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Acta Crystallogr Sect E Struct Rep Online. 2010 February 1; 66(Pt 2): m159.
Published online 2010 January 16. doi:  10.1107/S160053680905106X
PMCID: PMC2979685

Dipotassium diaqua­bis(methyl­enedi­phospho­nato-κ2 O,O′)cobaltate(II)

Abstract

In the title complex, K2[Co(CH4O6P2)2(H2O)2], the asymmetric unit contains two K+ cations and two half-anions in which the Co atoms lie on inversion centers. The CoII ions assume an octa­hedral CoO6 coordination geometry. In the crystal, a three-dimensional network is formed through O—H(...)O hydrogen-bond inter­actions as well as inter­molecular inter­actions between the K+ cations and neighbouring O atoms.

Related literature

For related structures, see: DeLaMatter et al. (1973 [triangle]); Jurisson et al. (1983 [triangle]); Barthelet et al. (2002 [triangle]); Stahl et al. (2006 [triangle]); Van der Merwe et al. (2009 [triangle]).

An external file that holds a picture, illustration, etc.
Object name is e-66-0m159-scheme1.jpg

Experimental

Crystal data

  • K2[Co(CH4O6P2)2(H2O)2]
  • M r = 521.13
  • Triclinic, An external file that holds a picture, illustration, etc.
Object name is e-66-0m159-efi1.jpg
  • a = 6.4523 (3) Å
  • b = 8.7056 (3) Å
  • c = 13.1930 (5) Å
  • α = 91.334 (2)°
  • β = 93.304 (2)°
  • γ = 93.333 (2)°
  • V = 738.32 (5) Å3
  • Z = 2
  • Mo Kα radiation
  • μ = 2.23 mm−1
  • T = 100 K
  • 0.28 × 0.17 × 0.17 mm

Data collection

  • Bruker X8 APEXII 4K Kappa CCD diffractometer
  • Absorption correction: multi-scan SADABS (Bruker, 2004 [triangle]) T min = 0.635, T max = 0.690
  • 13474 measured reflections
  • 3645 independent reflections
  • 3194 reflections with I > 2σ(I)
  • R int = 0.036

Refinement

  • R[F 2 > 2σ(F 2)] = 0.040
  • wR(F 2) = 0.1096
  • S = 1.23
  • 3645 reflections
  • 235parameters
  • 14 restraints
  • H atoms treated by a mixture of independent and constrained refinement
  • Δρmax = 1.04 e Å−3
  • Δρmin = −0.61 e Å−3

Data collection: APEX2 (Bruker, 2005 [triangle]); cell refinement: SAINT-Plus (Bruker, 2004 [triangle]); data reduction: SAINT-Plus and XPREP (Bruker, 2004 [triangle]); program(s) used to solve structure: SIR97 (Altomare et al., 1999 [triangle]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 [triangle]); molecular graphics: DIAMOND (Brandenburg & Putz, 2005 [triangle]); software used to prepare material for publication: WinGX (Farrugia, 1999 [triangle]).

Table 1
Selected bond lengths (Å)
Table 2
Hydrogen-bond geometry (Å, °)

Supplementary Material

Crystal structure: contains datablocks global, I. DOI: 10.1107/S160053680905106X/ds2013sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S160053680905106X/ds2013Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

Acknowledgments

The research fund of the University of the Free State is gratefully acknowledged.

supplementary crystallographic information

Comment

We reported a similar structure recently with the only differences being the cation and the +2 oxidation state of the cobalt ion (Van der Merwe et al.<i/>, 2009).

The CoIII ion in the title complex, K[Co(C2H4O6P)2(H2O)2], is in a slightly distorted octahedral environment with O–Co–O bond angles varying from 83.75 (10) to 96.25 (10)°. All the bonding distance and angles fall within the normal range observed for complexes of this nature. The P-O distances are significantly different for P═O and P-OH type bonds and vary from 1.501 (3) to 1.580 (3) Å. This could possibly be an indication that the assignment of positional disorders for the respective CoII complex previously was correct since these difference were not so prominent in the previous structure.

A three-dimensional network is provided by numerous hydrogen bonds and other weak interactions between the potassium ions and the oxygen atoms of the anionic species.

Experimental

CoCl2.6H2O (0,1696 g, 71 mmol) was dissolved in water (7 cm3) and heated to 70°C. Potassium bicarbonate was added to raise the pH to 5,5 after which methylene disphosphonate (0,25 g, 142 mmol), dissolved in water (5 cm3) was added dropwise. The final pH of the solution was adjusted to 1.50 to obtain the CoII salt as described previously (Van der Merwe et al.<i/> 2009). Crystals of the CoIII salt, suitable for X-ray diffraction, was obtained from redissolving and adding H2O2 to the solution.

Refinement

The aliphatic H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms with Uiso(H) = 1.2Ueq(C). The hydroxyl and aqua ions were located from the difference Fourier map. The highest residual electron density was located 1.40 Å from O1 and the deepest hole was 0.64 Å from Co1.

Figures

Fig. 1.
View of (I) (50% probability displacement ellipsoids). The potassium cations and hydrogen atoms have been omitted for clarity.

Crystal data

K2[Co(CH4O6P2)2(H2O)2]Z = 2
Mr = 521.13F(000) = 522
Triclinic, P1Dx = 2.344 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.4523 (3) ÅCell parameters from 5231 reflections
b = 8.7056 (3) Åθ = 2.1–28.3°
c = 13.1930 (5) ŵ = 2.23 mm1
α = 91.334 (2)°T = 100 K
β = 93.304 (2)°Cuboid, pink
γ = 93.333 (2)°0.28 × 0.17 × 0.17 mm
V = 738.32 (5) Å3

Data collection

Bruker X8 APEXII 4K Kappa CCD diffractometer3645 independent reflections
Radiation source: sealed tube3194 reflections with I > 2σ(I)
graphiteRint = 0.036
phi and ω scansθmax = 28.4°, θmin = 3.1°
Absorption correction: multi-scan SADABS (Bruker, 2004)h = −8→8
Tmin = 0.635, Tmax = 0.690k = −11→9
13474 measured reflectionsl = −16→17

Refinement

Refinement on F214 restraints
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.040w = 1/[σ2(Fo2) + (0.0164P)2 + 3.9058P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.096(Δ/σ)max < 0.001
S = 1.18Δρmax = 0.95 e Å3
3645 reflectionsΔρmin = −0.55 e Å3
235 parameters

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)

xyzUiso*/Ueq
C20.6164 (6)0.3660 (4)0.4121 (3)0.0083 (7)
H2A0.66470.46360.38520.01*
H2B0.49550.38440.45010.01*
O20.7149 (4)0.6643 (3)−0.06002 (19)0.0084 (5)
O10.4857 (4)0.6095 (3)0.1386 (2)0.0100 (5)
O40.3898 (4)0.8338 (3)0.2356 (2)0.0093 (5)
O50.7656 (4)0.7614 (3)0.2543 (2)0.0116 (5)
O61.0177 (4)0.7998 (3)0.0450 (2)0.0088 (5)
O80.6907 (4)−0.1647 (3)0.4464 (2)0.0137 (6)
O90.4598 (4)0.0840 (3)0.35124 (19)0.0087 (5)
O100.7627 (4)0.1422 (3)0.5352 (2)0.0109 (5)
O111.0208 (4)0.3123 (3)0.4451 (2)0.0091 (5)
O120.8299 (4)0.4173 (3)0.59244 (19)0.0097 (5)
O130.3411 (4)0.3121 (3)0.2569 (2)0.0094 (5)
O140.7069 (4)0.2216 (3)0.2347 (2)0.0105 (5)
P10.80660 (14)0.81239 (10)−0.00988 (7)0.00684 (18)
P20.57617 (14)0.76121 (11)0.18262 (7)0.00712 (18)
P30.53703 (14)0.23561 (10)0.30689 (7)0.00681 (18)
P40.81776 (14)0.30133 (11)0.49860 (7)0.00724 (18)
K10.08042 (13)0.57684 (9)0.19914 (6)0.01125 (17)
K20.02621 (13)0.04058 (10)0.31295 (7)0.01350 (18)
Co10.50.500.00676 (15)
Co20.500.50.00634 (15)
O70.8190 (4)0.9319 (3)−0.0975 (2)0.0092 (5)
O30.2452 (4)0.6119 (3)−0.0684 (2)0.0112 (5)
C10.6299 (6)0.8839 (4)0.0776 (3)0.0079 (7)
H1A0.49940.90060.04040.01*
H1B0.68640.98310.10480.01*
H8B0.778 (6)−0.215 (5)0.482 (3)0.02*
H8A0.699 (7)−0.185 (5)0.3838 (14)0.02*
H70.877 (7)1.020 (3)−0.081 (4)0.02*
H40.433 (8)0.911 (4)0.271 (3)0.02*
H130.332 (8)0.318 (6)0.1935 (15)0.02*
H3B0.175 (7)0.665 (5)−0.029 (3)0.02*
H3A0.266 (8)0.661 (5)−0.122 (2)0.02*
H120.872 (7)0.5089 (18)0.581 (2)0.02*

Atomic displacement parameters (Å2)

U11U22U33U12U13U23
C20.0098 (17)0.0062 (16)0.0087 (16)−0.0003 (13)−0.0010 (13)0.0003 (13)
O20.0098 (12)0.0077 (12)0.0073 (12)−0.0033 (10)0.0005 (10)0.0002 (9)
O10.0146 (13)0.0065 (12)0.0089 (12)−0.0016 (10)0.0035 (10)0.0000 (10)
O40.0087 (12)0.0097 (13)0.0092 (12)0.0009 (10)−0.0002 (10)−0.0023 (10)
O50.0108 (13)0.0146 (13)0.0095 (13)0.0031 (10)−0.0004 (10)−0.0010 (10)
O60.0082 (12)0.0078 (12)0.0102 (12)−0.0004 (9)−0.0006 (10)−0.0002 (10)
O80.0150 (14)0.0183 (14)0.0087 (13)0.0097 (11)−0.0005 (11)−0.0010 (11)
O90.0138 (13)0.0062 (12)0.0060 (12)−0.0009 (10)0.0005 (10)0.0016 (9)
O100.0088 (12)0.0092 (12)0.0146 (13)−0.0013 (10)−0.0011 (10)0.0065 (10)
O110.0084 (12)0.0096 (12)0.0092 (12)−0.0005 (10)0.0020 (10)0.0003 (10)
O120.0139 (13)0.0077 (12)0.0072 (12)−0.0016 (10)0.0002 (10)−0.0008 (10)
O130.0109 (13)0.0116 (13)0.0060 (12)0.0023 (10)−0.0004 (10)0.0006 (10)
O140.0118 (13)0.0127 (13)0.0075 (12)0.0023 (10)0.0023 (10)0.0021 (10)
P10.0077 (4)0.0062 (4)0.0067 (4)0.0000 (3)0.0006 (3)0.0005 (3)
P20.0080 (4)0.0076 (4)0.0059 (4)0.0014 (3)0.0010 (3)−0.0004 (3)
P30.0086 (4)0.0063 (4)0.0057 (4)0.0013 (3)0.0005 (3)0.0006 (3)
P40.0083 (4)0.0063 (4)0.0069 (4)−0.0006 (3)−0.0010 (3)0.0008 (3)
K10.0112 (4)0.0122 (4)0.0107 (4)0.0026 (3)0.0011 (3)0.0015 (3)
K20.0109 (4)0.0126 (4)0.0167 (4)0.0017 (3)−0.0022 (3)−0.0013 (3)
Co10.0083 (3)0.0060 (3)0.0061 (3)0.0004 (2)0.0010 (2)−0.0001 (2)
Co20.0072 (3)0.0061 (3)0.0058 (3)0.0001 (2)0.0008 (2)0.0007 (2)
O70.0137 (13)0.0055 (12)0.0081 (12)−0.0021 (10)0.0003 (10)0.0016 (10)
O30.0123 (13)0.0130 (13)0.0091 (13)0.0030 (10)0.0036 (10)0.0028 (10)
C10.0104 (17)0.0061 (16)0.0077 (16)0.0015 (13)0.0016 (13)0.0017 (13)

Geometric parameters (Å, °)

C2—P41.803 (4)O13—K13.018 (3)
C2—P31.804 (4)O13—K23.156 (3)
C2—H2A0.97O13—H130.837 (19)
C2—H2B0.97O14—P31.502 (3)
O2—P11.509 (3)O14—K2ii2.829 (3)
O1—Co12.052 (3)P1—O71.575 (3)
O2—Co12.132 (2)P1—C11.795 (4)
O3—Co12.127 (3)P2—C11.806 (4)
O1—P21.503 (3)K1—O12v2.776 (3)
O1—K12.779 (3)K1—O5vi2.780 (3)
O4—P21.581 (3)K1—O6vi2.871 (3)
O4—K12.922 (3)K1—O3vii3.023 (3)
O4—K2i3.235 (3)K1—O2viii3.153 (3)
O4—H40.84 (2)K2—O14vi2.829 (3)
O5—P21.501 (3)K2—O11vi2.909 (3)
O5—K1ii2.780 (3)K2—O10iv2.913 (3)
O5—K2iii2.936 (3)K2—O5ix2.936 (3)
O6—P11.516 (3)K2—O7viii3.076 (3)
O6—K1ii2.871 (3)K2—O4x3.235 (3)
O8—Co22.081 (3)K2—O8vi3.334 (3)
O8—K2ii3.334 (3)Co1—O1viii2.052 (3)
O8—H8B0.854 (19)Co1—O32.126 (3)
O8—H8A0.845 (19)Co1—O3viii2.126 (3)
O9—P31.525 (3)Co1—O2viii2.132 (2)
O9—Co22.117 (2)Co2—O10iv2.064 (3)
O9—K22.816 (3)Co2—O8iv2.081 (3)
O10—P41.508 (3)Co2—O9iv2.117 (2)
O10—Co22.064 (3)O7—K2viii3.076 (3)
O10—K2iv2.913 (3)O7—H70.849 (19)
O11—P41.523 (3)O3—K1vii3.023 (3)
O11—K2ii2.909 (3)O3—H3B0.855 (19)
O12—P41.575 (3)O3—H3A0.851 (19)
O12—K1v2.776 (3)C1—H1A0.97
O12—H120.848 (12)C1—H1B0.97
O13—P31.581 (3)
P4—C2—P3115.32 (19)P2vi—K1—H13153.4 (10)
P4—C2—H2A108.4Co1—K1—H1354.0 (7)
P3—C2—H2A108.4K2i—K1—H13146.4 (9)
P4—C2—H2B108.4O9—K2—O14vi135.52 (8)
P3—C2—H2B108.4O9—K2—O11vi83.20 (8)
H2A—C2—H2B107.5O9—K2—O10iv60.10 (7)
P1—O2—Co1127.62 (15)O9—K2—O5ix130.52 (8)
P2—O1—Co1133.27 (16)O9—K2—O7viii77.74 (7)
P2—O1—K1106.53 (13)O5ix—K2—O7viii91.81 (8)
Co1—O1—K1108.92 (11)O9—K2—O1349.14 (7)
P2—O4—K198.19 (12)O14vi—K2—O1386.68 (8)
P2—O4—H4110 (4)O11vi—K2—O1366.26 (7)
K1—O4—H4148 (4)O10iv—K2—O13107.66 (7)
K2i—O4—H466 (4)O5ix—K2—O13150.33 (8)
Co2—O8—H8B127 (3)O7viii—K2—O1358.52 (7)
K2ii—O8—H8B99 (3)O9—K2—O4x50.98 (7)
Co2—O8—H8A123 (3)O13—K2—O4x82.11 (7)
K2ii—O8—H8A60 (4)O9—K2—O8vi127.53 (8)
H8B—O8—H8A110 (3)O13—K2—O8vi159.31 (8)
P3—O9—Co2130.58 (16)O9—K2—P323.35 (5)
P3—O9—K2109.60 (13)O14vi—K2—P3112.35 (6)
Co2—O9—K2101.82 (10)O11vi—K2—P373.94 (6)
P4—O10—Co2129.21 (16)O10iv—K2—P382.69 (6)
P4—O12—H12115.7 (19)O5ix—K2—P3145.87 (6)
K1v—O12—H1298 (2)O7viii—K2—P366.54 (5)
P3—O13—K1155.08 (15)O13—K2—P325.79 (5)
P3—O13—K293.90 (12)O4x—K2—P364.15 (5)
K1—O13—K2106.16 (8)O8vi—K2—P3147.32 (6)
P3—O13—H13118 (4)O9—K2—P4vi103.51 (6)
K1—O13—H1371 (4)O13—K2—P4vi88.53 (5)
K2—O13—H13107 (4)P3—K2—P4vi97.09 (3)
O2—P1—O6114.49 (15)O9—K2—P3vi143.95 (6)
O2—P1—O7105.55 (15)P3—K2—P3vi124.45 (3)
O6—P1—O7111.05 (15)O1viii—Co1—O1180.00 (7)
O2—P1—C1109.75 (16)O1viii—Co1—O385.70 (11)
O6—P1—C1109.14 (16)O1—Co1—O394.30 (11)
O7—P1—C1106.53 (15)O1—Co1—O3viii85.70 (11)
O5—P2—O1118.26 (16)O3—Co1—O3viii180
O5—P2—O4111.00 (15)O1viii—Co1—O283.75 (10)
O1—P2—O4104.54 (15)O1—Co1—O296.25 (10)
O5—P2—C1109.50 (17)O3—Co1—O290.87 (10)
O1—P2—C1107.35 (16)O3viii—Co1—O289.13 (10)
O4—P2—C1105.35 (15)O1—Co1—O2viii83.75 (10)
O5—P2—K1130.08 (11)O3—Co1—O2viii89.13 (10)
O1—P2—K149.28 (11)O2—Co1—O2viii180
O4—P2—K155.38 (10)O1viii—Co1—K1138.32 (8)
C1—P2—K1120.38 (13)O1—Co1—K141.68 (8)
O14—P3—O9114.63 (15)O3—Co1—K169.01 (7)
O14—P3—O13112.37 (15)O3viii—Co1—K1110.99 (7)
O9—P3—O13107.36 (15)O2—Co1—K1127.38 (7)
O14—P3—C2111.63 (17)O2viii—Co1—K152.62 (7)
O9—P3—C2107.33 (16)O1—Co1—K1viii138.32 (8)
O13—P3—C2102.70 (15)O3—Co1—K1viii110.99 (7)
O14—P3—K2131.70 (12)O2—Co1—K1viii52.62 (7)
O9—P3—K247.05 (10)K1—Co1—K1viii180
O13—P3—K260.31 (10)O10iv—Co2—O10180
C2—P3—K2116.55 (12)O10iv—Co2—O891.42 (11)
O10—P4—O11113.25 (15)O10—Co2—O888.58 (11)
O10—P4—O12108.39 (15)O10—Co2—O8iv91.42 (11)
O11—P4—O12110.21 (15)O8—Co2—O8iv180.00 (14)
O10—P4—C2111.43 (16)O10iv—Co2—O986.68 (10)
O11—P4—C2107.68 (16)O10—Co2—O993.32 (10)
O12—P4—C2105.61 (16)O8—Co2—O989.71 (10)
O1—K1—O450.58 (7)O8iv—Co2—O990.29 (10)
O5vi—K1—O490.83 (8)O10—Co2—O9iv86.68 (10)
O6vi—K1—O471.15 (8)O8—Co2—O9iv90.29 (10)
O12v—K1—O1369.91 (8)O9—Co2—O9iv180.0000 (10)
O1—K1—O1366.27 (8)O10iv—Co2—K248.07 (7)
O5vi—K1—O13146.12 (8)O10—Co2—K2131.93 (7)
O6vi—K1—O13142.50 (8)O8—Co2—K2110.65 (8)
O4—K1—O1399.99 (8)O8iv—Co2—K269.35 (8)
O1—K1—P224.20 (6)O9—Co2—K245.66 (7)
O5vi—K1—P2116.53 (7)O9iv—Co2—K2134.34 (7)
O6vi—K1—P276.27 (6)O10—Co2—K2iv48.07 (7)
O4—K1—P226.43 (5)O8—Co2—K2iv69.35 (8)
O13—K1—P281.17 (6)O9—Co2—K2iv134.34 (7)
O1—K1—Co129.41 (6)K2—Co2—K2iv180.00 (2)
O5vi—K1—Co1146.14 (6)P1—O7—K2viii139.92 (14)
O6vi—K1—Co174.83 (5)P1—O7—H7116 (3)
O4—K1—Co176.27 (5)K2viii—O7—H790 (3)
O13—K1—Co167.68 (5)Co1—O3—K1vii118.88 (11)
O3vii—K1—Co190.27 (5)Co1—O3—H3B117 (3)
O2viii—K1—Co132.50 (5)K1vii—O3—H3B104 (3)
P2—K1—Co151.534 (19)Co1—O3—H3A118 (3)
O1—K1—H1359.5 (10)K1vii—O3—H3A85 (3)
O5vi—K1—H13159.3 (8)H3B—O3—H3A110 (3)
O6vi—K1—H13127.9 (5)P1—C1—P2115.47 (19)
O4—K1—H13102.4 (10)P1—C1—H1A108.4
O13—K1—H1316.1 (4)P2—C1—H1A108.4
O3vii—K1—H1387.6 (9)P1—C1—H1B108.4
O2viii—K1—H1334.1 (4)P2—C1—H1B108.4
P2—K1—H1379.2 (10)H1A—C1—H1B107.5

Symmetry codes: (i) x, y+1, z; (ii) x+1, y, z; (iii) x+1, y+1, z; (iv) −x+1, −y, −z+1; (v) −x+1, −y+1, −z+1; (vi) x−1, y, z; (vii) −x, −y+1, −z; (viii) −x+1, −y+1, −z; (ix) x−1, y−1, z; (x) x, y−1, z.

Hydrogen-bond geometry (Å, °)

D—H···AD—HH···AD···AD—H···A
O3—H3A···O14viii0.85 (2)1.83 (2)2.680 (4)175 (4)
O3—H3B···O6vi0.86 (2)1.89 (2)2.737 (4)172 (4)
O4—H4···O9i0.84 (2)1.81 (2)2.632 (4)166 (5)
O7—H7···O6xi0.85 (2)1.72 (2)2.570 (4)177 (5)
O8—H8A···O5x0.85 (2)1.84 (2)2.678 (4)170 (4)
O8—H8B···O11xii0.85 (2)1.84 (2)2.687 (4)176 (5)
O12—H12···O11xiii0.85 (1)1.72 (1)2.561 (4)175 (5)
O13—H13···O2viii0.84 (2)1.78 (2)2.616 (4)174 (5)

Symmetry codes: (viii) −x+1, −y+1, −z; (vi) x−1, y, z; (i) x, y+1, z; (xi) −x+2, −y+2, −z; (x) x, y−1, z; (xii) −x+2, −y, −z+1; (xiii) −x+2, −y+1, −z+1.

Footnotes

Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: DS2013).

References

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