In the title compound, Na
2[Co(C
3H
2O
4)
2(H
2O)
2]·H
2O, 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.
Supporting information
CCDC reference: 633666
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (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
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
top
Crystal data top
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) Å3 | Block, brown |
Z = 4 | 0.43 × 0.41 × 0.38 mm |
Data collection top
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 top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.041 | H-atom parameters constrained |
wR(F2) = 0.114 | w = 1/[σ2(Fo2) + (0.0723P)2 + 1.3726P] where P = (Fo2 + 2Fc2)/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 top
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 (Å2) top | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
C1—O2 | 1.235 (4) | Na1—H4 | 1.8837 |
C1—O1 | 1.261 (4) | Na2—O2viii | 2.418 (3) |
C1—C3 | 1.531 (5) | Na2—O2iii | 2.418 (3) |
C2—O4 | 1.245 (4) | Na2—O4v | 2.493 (3) |
C2—O3 | 1.267 (4) | Na2—O4ix | 2.493 (3) |
C2—C3 | 1.522 (4) | Na2—O7x | 2.6917 (8) |
C2—Na2i | 3.026 (4) | Na2—O7 | 2.6917 (8) |
C3—H1 | 0.9700 | Na2—O3v | 2.844 (3) |
C3—H2 | 0.9700 | Na2—O3ix | 2.844 (3) |
Co1—O6 | 1.595 (3) | Na2—C2v | 3.026 (4) |
Co1—O1ii | 1.995 (2) | Na2—C2ix | 3.026 (4) |
Co1—O1 | 1.995 (2) | Na2—Na1x | 3.2439 (11) |
Co1—O3ii | 2.016 (2) | O2—Na1xi | 2.321 (2) |
Co1—O3 | 2.016 (2) | O2—Na2xii | 2.418 (3) |
Co1—O5 | 2.219 (4) | O3—Na2i | 2.844 (3) |
Na1—O6 | 2.268 (4) | O4—Na2i | 2.493 (3) |
Na1—O2iii | 2.321 (2) | O4—Na1xiii | 2.507 (3) |
Na1—O2iv | 2.321 (2) | O5—H5 | 0.8459 |
Na1—O7 | 2.321 (3) | O6—H4 | 0.8590 |
Na1—O4v | 2.507 (3) | O7—Na2vii | 2.6917 (8) |
Na1—O4vi | 2.507 (3) | O7—H3 | 0.8502 |
Na1—Na2vii | 3.2439 (11) | | |
| | | |
O2—C1—O1 | 122.8 (3) | O4ix—Na2—O7x | 78.27 (8) |
O2—C1—C3 | 119.2 (3) | O2viii—Na2—O7 | 87.19 (8) |
O1—C1—C3 | 117.9 (3) | O2iii—Na2—O7 | 76.72 (9) |
O4—C2—O3 | 121.4 (3) | O4v—Na2—O7 | 78.27 (8) |
O4—C2—C3 | 119.9 (3) | O4ix—Na2—O7 | 116.70 (9) |
O3—C2—C3 | 118.6 (3) | O7x—Na2—O7 | 155.88 (8) |
O4—C2—Na2i | 53.41 (18) | O2viii—Na2—O3v | 146.64 (8) |
O3—C2—Na2i | 69.59 (18) | O2iii—Na2—O3v | 92.55 (9) |
C3—C2—Na2i | 162.7 (2) | O4v—Na2—O3v | 47.92 (8) |
C2—C3—C1 | 111.7 (3) | O4ix—Na2—O3v | 83.90 (9) |
C2—C3—H1 | 109.3 | O7x—Na2—O3v | 71.65 (7) |
C1—C3—H1 | 109.3 | O7—Na2—O3v | 126.17 (7) |
C2—C3—H2 | 109.3 | O2viii—Na2—O3ix | 92.55 (9) |
C1—C3—H2 | 109.3 | O2iii—Na2—O3ix | 146.64 (8) |
H1—C3—H2 | 107.9 | O4v—Na2—O3ix | 83.90 (9) |
O6—Co1—O1ii | 98.32 (9) | O4ix—Na2—O3ix | 47.92 (8) |
O6—Co1—O1 | 98.32 (9) | O7x—Na2—O3ix | 126.17 (7) |
O1ii—Co1—O1 | 163.36 (18) | O7—Na2—O3ix | 71.65 (6) |
O6—Co1—O3ii | 100.25 (7) | O3v—Na2—O3ix | 97.53 (11) |
O1ii—Co1—O3ii | 88.62 (11) | O2viii—Na2—C2v | 170.76 (9) |
O1—Co1—O3ii | 88.43 (11) | O2iii—Na2—C2v | 88.62 (9) |
O6—Co1—O3 | 100.25 (7) | O4v—Na2—C2v | 23.64 (9) |
O1ii—Co1—O3 | 88.43 (11) | O4ix—Na2—C2v | 93.79 (10) |
O1—Co1—O3 | 88.62 (11) | O7x—Na2—C2v | 95.77 (8) |
O3ii—Co1—O3 | 159.50 (15) | O7—Na2—C2v | 101.59 (8) |
O6—Co1—O5 | 180.0 | O3v—Na2—C2v | 24.68 (8) |
O1ii—Co1—O5 | 81.68 (9) | O3ix—Na2—C2v | 87.56 (9) |
O1—Co1—O5 | 81.68 (9) | O2viii—Na2—C2ix | 88.62 (9) |
O3ii—Co1—O5 | 79.75 (7) | O2iii—Na2—C2ix | 170.76 (9) |
O3—Co1—O5 | 79.75 (7) | O4v—Na2—C2ix | 93.79 (10) |
O6—Na1—O2iii | 93.59 (8) | O4ix—Na2—C2ix | 23.64 (9) |
O6—Na1—O2iv | 93.59 (8) | O7x—Na2—C2ix | 101.59 (8) |
O2iii—Na1—O2iv | 172.83 (17) | O7—Na2—C2ix | 95.77 (8) |
O6—Na1—O7 | 180.0 | O3v—Na2—C2ix | 87.56 (9) |
O2iii—Na1—O7 | 86.41 (8) | O3ix—Na2—C2ix | 24.68 (8) |
O2iv—Na1—O7 | 86.41 (8) | C2v—Na2—C2ix | 87.64 (13) |
O6—Na1—O4v | 94.65 (7) | O2viii—Na2—Na1x | 45.56 (6) |
O2iii—Na1—O4v | 81.08 (9) | O2iii—Na2—Na1x | 117.96 (8) |
O2iv—Na1—O4v | 98.33 (9) | O4v—Na2—Na1x | 148.26 (8) |
O7—Na1—O4v | 85.35 (7) | O4ix—Na2—Na1x | 49.74 (6) |
O6—Na1—O4vi | 94.65 (7) | O7x—Na2—Na1x | 44.86 (7) |
O2iii—Na1—O4vi | 98.33 (9) | O7—Na2—Na1x | 129.53 (7) |
O2iv—Na1—O4vi | 81.08 (9) | O3v—Na2—Na1x | 102.34 (6) |
O7—Na1—O4vi | 85.35 (7) | O3ix—Na2—Na1x | 90.84 (5) |
O4v—Na1—O4vi | 170.71 (15) | C2v—Na2—Na1x | 125.20 (7) |
O6—Na1—Na2vii | 125.13 (2) | C2ix—Na2—Na1x | 70.96 (6) |
O2iii—Na1—Na2vii | 126.61 (9) | C1—O1—Co1 | 126.5 (2) |
O2iv—Na1—Na2vii | 48.06 (7) | C1—O2—Na1xi | 145.7 (2) |
O7—Na1—Na2vii | 54.87 (2) | C1—O2—Na2xii | 127.7 (2) |
O4v—Na1—Na2vii | 123.93 (8) | Na1xi—O2—Na2xii | 86.38 (9) |
O4vi—Na1—Na2vii | 49.35 (7) | C2—O3—Co1 | 125.6 (2) |
O6—Na1—H4 | 21.4 | C2—O3—Na2i | 85.74 (18) |
O2iii—Na1—H4 | 88.0 | Co1—O3—Na2i | 141.74 (11) |
O2iv—Na1—H4 | 98.7 | C2—O4—Na2i | 102.9 (2) |
O7—Na1—H4 | 158.6 | C2—O4—Na1xiii | 150.6 (2) |
O4v—Na1—H4 | 114.2 | Na2i—O4—Na1xiii | 80.90 (9) |
O4vi—Na1—H4 | 75.0 | Co1—O5—H5 | 125.4 |
Na2vii—Na1—H4 | 114.3 | Co1—O6—Na1 | 180.0 |
O2viii—Na2—O2iii | 96.29 (15) | Co1—O6—H4 | 126.8 |
O2viii—Na2—O4v | 165.42 (9) | Na1—O6—H4 | 53.2 |
O2iii—Na2—O4v | 79.52 (9) | Na1—O7—Na2vii | 80.27 (7) |
O2viii—Na2—O4ix | 79.52 (9) | Na1—O7—Na2 | 80.27 (7) |
O2iii—Na2—O4ix | 165.42 (9) | Na2vii—O7—Na2 | 160.54 (13) |
O4v—Na2—O4ix | 107.84 (15) | Na1—O7—H3 | 123.6 |
O2viii—Na2—O7x | 76.72 (9) | Na2vii—O7—H3 | 97.6 |
O2iii—Na2—O7x | 87.19 (8) | Na2—O7—H3 | 93.1 |
O4v—Na2—O7x | 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) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O4xiv | 0.85 | 1.90 | 2.743 (4) | 176 |
O7—H3···O1viii | 0.85 | 1.98 | 2.797 (3) | 162 |
Symmetry codes: (viii) x+1/2, y+1/2, z; (xiv) x, −y, −z+1. |