Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The crystal structure of the title compound, CoK2(H2P2O7)2·2H2O, is, to our knowledge, the first example of a mixed-metal di­hydrogendiphosphate, containing an alkali earth metal and a divalent transition metal. The metal ions and the two water O atoms are located on a crystallographic mirror plane.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802016161/br6060sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802016161/br6060Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](P-O) = 0.001 Å
  • R factor = 0.024
  • wR factor = 0.061
  • Data-to-parameter ratio = 19.1

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
DIFF_019 Alert A _diffrn_standards_number is missing Number of standards used in measurement.
Author response: The data were measured on an area-detector.
DIFF_020  Alert A _diffrn_standards_interval_count and
          _diffrn_standards_interval_time are missing. Number of measurements
          between standards or time (min) between standards.
Author response: The data were measured on an area-detector.
DIFF_022  Alert A _diffrn_standards_decay_% is missing
          Percentage decrease in standards intensity.
Author response: The data were measured on an area-detector.

3 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
0 Alert Level C = Please check

Comment top

The crystal structure of the title compound, CoK2(H2P2O7)2.2H2O, is to our knowledge the first example of a mixed-metal dihydrogendiphosphate, containing an alkaline and a divalent transition metal. The metal atoms and the two water oxygen atoms are located on a crystallographic mirror plane. The Co atoms are octahedrally coordinated. Whereas one of the K ions (K1) is bonded to seven O atoms, the other one (K2) makes eight bonds to O atoms.

Experimental top

Crystals were prepared by dissolving stochiometric amounts of CoCl2.6 H2O in a solution made of K4P2O7 in distilled water. The mixture has been stirred for 1 d and the resulting light-pink solution was allowed to stand at atmospheric temperature. After two to three weeks, pink crystals deposited which have been filtered off and washed with a solution of ethanol (80%).

Refinement top

All H atoms could be located by difference Fourier synthesis and were refined isotropically.

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991).

Figures top
[Figure 1] Fig. 1. Perspective view of the title compound with the atom numbering; displacement ellipsoids are at the 50% probability level. Symmetry operators for generating equivalent atoms: (i) x, 1/2 − y, z; (ii) x, 3/2 − y, z; (iii) −1/2 + x, y, 1/2 − z; (iv) −1/2 + x, 1 − y, −1/2 + z; (v) 1/2 − x, −1/2 + y, −1/2 + z; (vi) −1/2 + x, 1/2 − y, 1/2 − z; (vii) −x, −1/2 + y, 1 − z; (viii) −x, 1 − y, 1 − z; (ix) 1/2 − x, −1/2 + y, 1/2 + z; (x) 1/2 − x, 1 − y, 1/2 + z.
(I) top
Crystal data top
[CoK2(H2P2O7)2]·2H2OF(000) = 1044
Mr = 525.07Dx = 2.439 Mg m3
Orthorhombic, PnmaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2nCell parameters from 28672 reflections
a = 9.7044 (5) Åθ = 3.6–31.3°
b = 11.0023 (6) ŵ = 2.32 mm1
c = 13.3937 (8) ÅT = 173 K
V = 1430.05 (14) Å3Block, light pink
Z = 40.22 × 0.18 × 0.09 mm
Data collection top
STOE IPDS II two-circle
diffractometer
2441 independent reflections
Radiation source: fine-focus sealed tube2173 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.049
ω scansθmax = 31.4°, θmin = 3.7°
Absorption correction: multi-scan
(MULABS; Spek, 1990; Blessing, 1995)
h = 1114
Tmin = 0.630, Tmax = 0.819k = 1616
24419 measured reflectionsl = 1919
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.061All H-atom parameters refined
S = 1.03 w = 1/[σ2(Fo2) + (0.0413P)2 + 0.057P]
where P = (Fo2 + 2Fc2)/3
2441 reflections(Δ/σ)max = 0.001
128 parametersΔρmax = 0.37 e Å3
0 restraintsΔρmin = 0.70 e Å3
Crystal data top
[CoK2(H2P2O7)2]·2H2OV = 1430.05 (14) Å3
Mr = 525.07Z = 4
Orthorhombic, PnmaMo Kα radiation
a = 9.7044 (5) ŵ = 2.32 mm1
b = 11.0023 (6) ÅT = 173 K
c = 13.3937 (8) Å0.22 × 0.18 × 0.09 mm
Data collection top
STOE IPDS II two-circle
diffractometer
2441 independent reflections
Absorption correction: multi-scan
(MULABS; Spek, 1990; Blessing, 1995)
2173 reflections with I > 2σ(I)
Tmin = 0.630, Tmax = 0.819Rint = 0.049
24419 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0240 restraints
wR(F2) = 0.061All H-atom parameters refined
S = 1.03Δρmax = 0.37 e Å3
2441 reflectionsΔρmin = 0.70 e Å3
128 parameters
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
xyzUiso*/Ueq
Co10.33245 (3)0.75000.359996 (17)0.01247 (7)
K10.24827 (4)0.25000.12438 (3)0.01874 (9)
K20.05369 (5)0.25000.60189 (3)0.02236 (10)
P10.43938 (3)0.48215 (3)0.27784 (2)0.01280 (7)
P20.24459 (3)0.48399 (3)0.44235 (2)0.01275 (7)
O10.42720 (11)0.42671 (10)0.17638 (7)0.01901 (19)
O20.44669 (10)0.61916 (9)0.28249 (7)0.01586 (17)
O30.56475 (12)0.42715 (10)0.33434 (8)0.01954 (19)
H30.589 (4)0.473 (3)0.375 (2)0.055 (9)*
O40.30435 (11)0.43772 (9)0.33644 (7)0.01684 (18)
O50.11138 (11)0.40773 (9)0.45315 (7)0.01637 (18)
H50.057 (3)0.416 (3)0.413 (2)0.040 (7)*
O60.21535 (11)0.61816 (9)0.43337 (7)0.01678 (18)
O70.34367 (11)0.44641 (10)0.52279 (7)0.01930 (19)
O80.19631 (16)0.75000.23301 (11)0.0184 (3)
H80.141 (3)0.803 (3)0.223 (2)0.052 (9)*
O90.47828 (16)0.75000.47601 (10)0.0169 (3)
H90.536 (3)0.808 (2)0.4789 (19)0.042 (7)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.01200 (12)0.01229 (11)0.01314 (11)0.0000.00057 (8)0.000
K10.01607 (19)0.01573 (17)0.02441 (18)0.0000.00209 (14)0.000
K20.0310 (2)0.02212 (19)0.01395 (16)0.0000.00207 (15)0.000
P10.01289 (15)0.01317 (14)0.01234 (13)0.00020 (11)0.00038 (10)0.00072 (9)
P20.01209 (15)0.01346 (15)0.01269 (13)0.00059 (11)0.00006 (10)0.00065 (9)
O10.0176 (5)0.0248 (5)0.0146 (4)0.0050 (4)0.0017 (3)0.0048 (3)
O20.0157 (4)0.0139 (4)0.0179 (4)0.0006 (3)0.0021 (3)0.0007 (3)
O30.0194 (5)0.0188 (4)0.0204 (4)0.0043 (4)0.0039 (4)0.0018 (4)
O40.0180 (5)0.0171 (4)0.0155 (4)0.0037 (4)0.0031 (3)0.0018 (3)
O50.0144 (4)0.0187 (4)0.0160 (4)0.0034 (3)0.0009 (3)0.0037 (3)
O60.0171 (4)0.0143 (4)0.0189 (4)0.0008 (3)0.0036 (3)0.0017 (3)
O70.0179 (5)0.0220 (5)0.0180 (4)0.0031 (4)0.0056 (3)0.0014 (3)
O80.0163 (7)0.0175 (6)0.0215 (6)0.0000.0046 (5)0.000
O90.0162 (6)0.0159 (6)0.0187 (6)0.0000.0029 (5)0.000
Geometric parameters (Å, º) top
Co1—O6i2.0883 (10)K2—O6iv3.0239 (12)
Co1—O62.0883 (10)K2—O8iv3.2827 (17)
Co1—O2i2.0926 (10)K2—Co1ii3.6293 (5)
Co1—O22.0926 (10)K2—P1ii3.7740 (4)
Co1—O92.1018 (14)K2—P1ix3.7740 (4)
Co1—O82.1537 (15)K2—Co1iv3.7819 (6)
Co1—K1ii3.6266 (5)P1—O11.4942 (10)
Co1—K2iii3.6293 (5)P1—O21.5103 (10)
Co1—K2iv3.7818 (6)P1—O31.5553 (11)
K1—O3v2.6975 (11)P1—O41.6038 (11)
K1—O3vi2.6975 (11)P1—K2iii3.7740 (4)
K1—O12.6982 (11)P2—O71.5021 (10)
K1—O1vii2.6982 (11)P2—O61.5079 (11)
K1—O6viii2.9621 (10)P2—O51.5479 (11)
K1—O6iii2.9621 (10)P2—O41.6149 (10)
K1—O9iii2.9636 (16)P2—K1ii3.8097 (5)
K1—Co1iii3.6267 (5)O2—K2iii2.8149 (10)
K1—P1vii3.7667 (5)O3—K1xi2.6975 (11)
K1—P13.7667 (5)O3—H30.78 (3)
K1—P2viii3.8097 (5)O5—H50.76 (3)
K1—P2iii3.8097 (5)O6—K1ii2.9621 (10)
K2—O52.7007 (10)O6—K2iv3.0239 (12)
K2—O5vii2.7008 (10)O8—K2iii2.9951 (17)
K2—O2ii2.8149 (10)O8—K2iv3.2826 (17)
K2—O2ix2.8149 (10)O8—H80.81 (3)
K2—O8ii2.9951 (17)O9—K1ii2.9635 (16)
K2—O6x3.0239 (12)O9—H90.85 (3)
O6i—Co1—O687.99 (6)O2ii—K2—O8ii59.81 (3)
O6i—Co1—O2i92.51 (4)O2ix—K2—O8ii59.81 (3)
O6—Co1—O2i178.28 (4)O5—K2—O6x111.84 (3)
O6i—Co1—O2178.28 (4)O5vii—K2—O6x75.85 (3)
O6—Co1—O292.51 (4)O2ii—K2—O6x112.23 (3)
O2i—Co1—O286.93 (5)O2ix—K2—O6x83.55 (3)
O6i—Co1—O991.06 (4)O8ii—K2—O6x142.28 (3)
O6—Co1—O991.06 (4)O5—K2—O6iv75.85 (3)
O2i—Co1—O990.57 (4)O5vii—K2—O6iv111.84 (3)
O2—Co1—O990.57 (4)O2ii—K2—O6iv83.55 (3)
O6i—Co1—O892.17 (4)O2ix—K2—O6iv112.23 (3)
O6—Co1—O892.17 (4)O8ii—K2—O6iv142.28 (3)
O2i—Co1—O886.17 (4)O6x—K2—O6iv57.33 (4)
O2—Co1—O886.17 (4)O5—K2—O8iv130.55 (3)
O9—Co1—O8175.51 (6)O5vii—K2—O8iv130.55 (3)
O6i—Co1—K1ii54.76 (3)O2ii—K2—O8iv54.56 (3)
O6—Co1—K1ii54.76 (3)O2ix—K2—O8iv54.56 (3)
O2i—Co1—K1ii126.78 (3)O8ii—K2—O8iv101.752 (13)
O2—Co1—K1ii126.78 (3)O6x—K2—O8iv57.80 (3)
O9—Co1—K1ii54.80 (4)O6iv—K2—O8iv57.80 (3)
O8—Co1—K1ii129.69 (4)O5—K2—Co1ii129.76 (2)
O6i—Co1—K2iii127.87 (3)O5vii—K2—Co1ii129.76 (2)
O6—Co1—K2iii127.87 (3)O2ii—K2—Co1ii35.10 (2)
O2i—Co1—K2iii50.67 (3)O2ix—K2—Co1ii35.10 (2)
O2—Co1—K2iii50.67 (3)O8ii—K2—Co1ii36.37 (3)
O9—Co1—K2iii119.95 (4)O6x—K2—Co1ii114.31 (2)
O8—Co1—K2iii55.57 (4)O6iv—K2—Co1ii114.31 (2)
K1ii—Co1—K2iii174.749 (13)O8iv—K2—Co1ii65.38 (3)
O6i—Co1—K2iv52.94 (3)O5—K2—P1ii87.43 (2)
O6—Co1—K2iv52.94 (3)O5vii—K2—P1ii163.47 (3)
O2i—Co1—K2iv126.29 (3)O2ii—K2—P1ii20.62 (2)
O2—Co1—K2iv126.29 (3)O2ix—K2—P1ii82.11 (2)
O9—Co1—K2iv124.57 (4)O8ii—K2—P1ii67.630 (17)
O8—Co1—K2iv59.92 (4)O6x—K2—P1ii119.18 (2)
K1ii—Co1—K2iv69.768 (10)O6iv—K2—P1ii74.83 (2)
K2iii—Co1—K2iv115.483 (12)O8iv—K2—P1ii65.953 (16)
O3v—K1—O3vi92.53 (5)Co1ii—K2—P1ii53.114 (7)
O3v—K1—O1153.20 (4)O5—K2—P1ix163.47 (3)
O3vi—K1—O181.45 (4)O5vii—K2—P1ix87.43 (2)
O3v—K1—O1vii81.45 (4)O2ii—K2—P1ix82.11 (2)
O3vi—K1—O1vii153.20 (4)O2ix—K2—P1ix20.62 (2)
O1—K1—O1vii92.20 (5)O8ii—K2—P1ix67.630 (17)
O3v—K1—O6viii84.37 (3)O6x—K2—P1ix74.83 (2)
O3vi—K1—O6viii127.56 (3)O6iv—K2—P1ix119.18 (2)
O1—K1—O6viii119.94 (3)O8iv—K2—P1ix65.953 (16)
O1vii—K1—O6viii78.08 (3)Co1ii—K2—P1ix53.114 (7)
O3v—K1—O6iii127.56 (3)P1ii—K2—P1ix102.680 (14)
O3vi—K1—O6iii84.37 (3)O5—K2—Co1iv107.76 (3)
O1—K1—O6iii78.08 (3)O5vii—K2—Co1iv107.76 (3)
O1vii—K1—O6iii119.94 (3)O2ii—K2—Co1iv83.26 (2)
O6viii—K1—O6iii58.64 (4)O2ix—K2—Co1iv83.26 (2)
O3v—K1—O9iii69.37 (3)O8ii—K2—Co1iv136.34 (3)
O3vi—K1—O9iii69.37 (3)O6x—K2—Co1iv33.443 (19)
O1—K1—O9iii130.58 (3)O6iv—K2—Co1iv33.44 (2)
O1vii—K1—O9iii130.58 (3)O8iv—K2—Co1iv34.59 (3)
O6viii—K1—O9iii60.61 (3)Co1ii—K2—Co1iv99.967 (11)
O6iii—K1—O9iii60.61 (3)P1ii—K2—Co1iv86.179 (10)
O3v—K1—Co1iii93.30 (3)P1ix—K2—Co1iv86.179 (10)
O3vi—K1—Co1iii93.30 (3)O1—P1—O2116.66 (6)
O1—K1—Co1iii113.02 (2)O1—P1—O3110.22 (6)
O1vii—K1—Co1iii113.02 (2)O2—P1—O3109.36 (6)
O6viii—K1—Co1iii35.16 (2)O1—P1—O4104.83 (6)
O6iii—K1—Co1iii35.16 (2)O2—P1—O4108.81 (6)
O9iii—K1—Co1iii35.42 (3)O3—P1—O4106.41 (6)
O3v—K1—P1vii73.93 (3)O2—P1—K1136.25 (4)
O3vi—K1—P1vii134.68 (3)O3—P1—K1112.76 (4)
O1—K1—P1vii91.77 (3)O4—P1—K170.01 (4)
O1vii—K1—P1vii18.86 (2)O1—P1—K2iii75.66 (4)
O6viii—K1—P1vii94.62 (2)O3—P1—K2iii126.42 (5)
O6iii—K1—P1vii138.13 (3)O4—P1—K2iii123.93 (4)
O9iii—K1—P1vii136.985 (8)K1—P1—K2iii101.393 (11)
Co1iii—K1—P1vii129.729 (9)O7—P2—O6116.56 (6)
O3v—K1—P1134.68 (3)O7—P2—O5108.56 (6)
O3vi—K1—P173.93 (3)O6—P2—O5112.39 (6)
O1—K1—P118.86 (2)O7—P2—O4108.26 (6)
O1vii—K1—P191.77 (3)O6—P2—O4107.82 (5)
O6viii—K1—P1138.13 (3)O5—P2—O4102.19 (5)
O6iii—K1—P194.62 (2)O7—P2—K1ii74.98 (4)
O9iii—K1—P1136.984 (8)O5—P2—K1ii111.83 (4)
Co1iii—K1—P1129.729 (9)O4—P2—K1ii142.92 (4)
P1vii—K1—P185.389 (14)O7—P2—K273.98 (5)
O3v—K1—P2viii65.68 (2)O6—P2—K2127.76 (4)
O3vi—K1—P2viii134.29 (3)O4—P2—K2116.91 (4)
O1—K1—P2viii135.00 (3)K1ii—P2—K299.695 (11)
O1vii—K1—P2viii66.42 (2)P1—O1—K1125.44 (6)
O6viii—K1—P2viii21.40 (2)P1—O2—Co1133.01 (6)
O6iii—K1—P2viii79.71 (2)P1—O2—K2iii118.35 (5)
O9iii—K1—P2viii65.442 (17)Co1—O2—K2iii94.23 (4)
Co1iii—K1—P2viii51.618 (7)P1—O3—K1xi153.81 (6)
P1vii—K1—P2viii79.592 (8)P1—O3—H3109 (3)
P1—K1—P2viii149.449 (14)K1xi—O3—H397 (3)
O3v—K1—P2iii134.29 (3)P1—O4—P2128.85 (6)
O3vi—K1—P2iii65.68 (2)P2—O5—K2126.18 (5)
O1—K1—P2iii66.42 (2)P2—O5—H5116 (2)
O1vii—K1—P2iii135.00 (3)K2—O5—H5117 (2)
O6viii—K1—P2iii79.71 (2)P2—O6—Co1127.96 (6)
O6iii—K1—P2iii21.40 (2)P2—O6—K1ii112.83 (5)
O9iii—K1—P2iii65.442 (17)Co1—O6—K1ii90.08 (4)
Co1iii—K1—P2iii51.618 (7)P2—O6—K2iv130.13 (6)
P1vii—K1—P2iii149.448 (14)Co1—O6—K2iv93.62 (4)
P1—K1—P2iii79.591 (8)K1ii—O6—K2iv90.16 (3)
P2viii—K1—P2iii100.388 (14)Co1—O8—K2iii88.06 (5)
O5—K2—O5vii79.97 (4)Co1—O8—K2iv85.49 (5)
O5—K2—O2ii107.79 (3)K2iii—O8—K2iv173.55 (5)
O5vii—K2—O2ii164.32 (3)Co1—O8—H8123 (2)
O5—K2—O2ix164.32 (3)K2iii—O8—H8116 (2)
O5vii—K2—O2ix107.79 (3)K2iv—O8—H867 (2)
O2ii—K2—O2ix61.52 (4)Co1—O9—K1ii89.78 (5)
O5—K2—O8ii105.34 (3)Co1—O9—H9118.5 (18)
O5vii—K2—O8ii105.34 (3)K1ii—O9—H9117.2 (18)
O3v—K1—P1—O1171.35 (8)O4—P1—O1—K112.95 (9)
O3vi—K1—P1—O1111.38 (8)K2iii—P1—O1—K1134.84 (7)
O1vii—K1—P1—O191.64 (9)O3v—K1—O1—P113.73 (13)
O6viii—K1—P1—O117.61 (8)O3vi—K1—O1—P164.81 (7)
O6iii—K1—P1—O128.60 (8)O1vii—K1—O1—P189.02 (8)
O9iii—K1—P1—O179.17 (9)O6viii—K1—O1—P1166.53 (6)
Co1iii—K1—P1—O130.67 (8)O6iii—K1—O1—P1150.82 (8)
P1vii—K1—P1—O1109.39 (8)O9iii—K1—O1—P1118.09 (8)
P2viii—K1—P1—O148.95 (8)Co1iii—K1—O1—P1154.77 (6)
P2iii—K1—P1—O143.89 (8)P1vii—K1—O1—P170.16 (7)
O3v—K1—P1—O2118.65 (7)P2viii—K1—O1—P1147.18 (6)
O3vi—K1—P1—O241.37 (6)P2iii—K1—O1—P1131.93 (8)
O1—K1—P1—O270.01 (9)O1—P1—O2—Co1125.99 (8)
O1vii—K1—P1—O2161.64 (6)O3—P1—O2—Co1108.12 (9)
O6viii—K1—P1—O287.62 (7)O4—P1—O2—Co17.72 (10)
O6iii—K1—P1—O241.41 (6)K1—P1—O2—Co188.13 (8)
O9iii—K1—P1—O29.17 (8)K2iii—P1—O2—Co1128.17 (11)
Co1iii—K1—P1—O239.34 (6)O1—P1—O2—K2iii2.19 (8)
P1vii—K1—P1—O2179.40 (6)O3—P1—O2—K2iii123.70 (6)
P2viii—K1—P1—O2118.95 (6)O4—P1—O2—K2iii120.46 (6)
P2iii—K1—P1—O226.12 (6)K1—P1—O2—K2iii40.04 (8)
O3v—K1—P1—O377.99 (4)O6—Co1—O2—P13.25 (9)
O3vi—K1—P1—O3155.27 (5)O2i—Co1—O2—P1175.12 (5)
O1—K1—P1—O393.35 (9)O9—Co1—O2—P194.34 (8)
O1vii—K1—P1—O31.71 (5)O8—Co1—O2—P188.75 (8)
O6viii—K1—P1—O375.74 (6)K1ii—Co1—O2—P149.76 (9)
O6iii—K1—P1—O3121.95 (5)K2iii—Co1—O2—P1136.07 (10)
O9iii—K1—P1—O3172.52 (6)K2iv—Co1—O2—P141.01 (9)
Co1iii—K1—P1—O3124.02 (5)O6—Co1—O2—K2iii139.33 (4)
P1vii—K1—P1—O316.04 (5)O2i—Co1—O2—K2iii39.04 (5)
P2viii—K1—P1—O344.41 (5)O9—Co1—O2—K2iii129.59 (4)
P2iii—K1—P1—O3137.24 (5)O8—Co1—O2—K2iii47.32 (4)
O3v—K1—P1—O421.98 (6)K1ii—Co1—O2—K2iii174.167 (15)
O3vi—K1—P1—O455.29 (5)K2iv—Co1—O2—K2iii95.07 (3)
O1—K1—P1—O4166.67 (9)O1—P1—O3—K1xi27.81 (17)
O1vii—K1—P1—O4101.69 (5)O2—P1—O3—K1xi157.31 (14)
O6viii—K1—P1—O4175.72 (5)O4—P1—O3—K1xi85.32 (15)
O6iii—K1—P1—O4138.07 (5)K1—P1—O3—K1xi10.57 (16)
O9iii—K1—P1—O487.50 (6)K2iii—P1—O3—K1xi114.58 (14)
Co1iii—K1—P1—O4136.00 (4)O1—P1—O4—P2168.82 (8)
P1vii—K1—P1—O483.94 (4)O2—P1—O4—P243.33 (10)
P2viii—K1—P1—O4144.38 (5)O3—P1—O4—P274.40 (10)
P2iii—K1—P1—O4122.78 (4)K1—P1—O4—P2176.82 (9)
O3v—K1—P1—K2iii144.17 (4)K2iii—P1—O4—P286.33 (9)
O3vi—K1—P1—K2iii66.89 (3)O7—P2—O4—P167.36 (10)
O1—K1—P1—K2iii44.49 (8)O6—P2—O4—P159.55 (10)
O1vii—K1—P1—K2iii136.12 (2)O5—P2—O4—P1178.16 (8)
O6viii—K1—P1—K2iii62.10 (3)K1ii—P2—O4—P121.72 (13)
O6iii—K1—P1—K2iii15.89 (2)K2—P2—O4—P1148.25 (7)
O9iii—K1—P1—K2iii34.68 (5)O7—P2—O5—K25.81 (8)
Co1iii—K1—P1—K2iii13.819 (19)O6—P2—O5—K2124.62 (6)
P1vii—K1—P1—K2iii153.882 (10)O4—P2—O5—K2120.06 (7)
P2viii—K1—P1—K2iii93.43 (2)K1ii—P2—O5—K274.98 (6)
P2iii—K1—P1—K2iii0.599 (12)O5vii—K2—O5—P2105.26 (6)
O5—K2—P2—O7174.27 (8)O2ii—K2—O5—P260.69 (7)
O5vii—K2—P2—O7101.89 (5)O2ix—K2—O5—P215.93 (17)
O2ii—K2—P2—O762.67 (5)O8ii—K2—O5—P21.95 (7)
O2ix—K2—P2—O713.27 (6)O6x—K2—O5—P2175.48 (6)
O8ii—K2—P2—O73.84 (5)O6iv—K2—O5—P2139.01 (7)
O6x—K2—P2—O7168.72 (5)O8iv—K2—O5—P2118.89 (7)
O6iv—K2—P2—O7146.23 (5)Co1ii—K2—O5—P228.98 (8)
O8iv—K2—P2—O7107.17 (6)P1ii—K2—O5—P264.01 (7)
Co1ii—K2—P2—O729.53 (4)P1ix—K2—O5—P264.40 (13)
P1ii—K2—P2—O771.77 (4)Co1iv—K2—O5—P2149.16 (6)
P1ix—K2—P2—O725.13 (5)O7—P2—O6—Co182.29 (8)
Co1iv—K2—P2—O7149.79 (4)O5—P2—O6—Co1151.49 (7)
O5—K2—P2—O674.26 (9)O4—P2—O6—Co139.63 (9)
O5vii—K2—P2—O6146.64 (6)K1ii—P2—O6—Co1109.30 (9)
O2ii—K2—P2—O648.79 (6)K2—P2—O6—Co1172.11 (4)
O2ix—K2—P2—O698.19 (7)O7—P2—O6—K1ii27.01 (8)
O8ii—K2—P2—O6107.62 (6)O5—P2—O6—K1ii99.22 (6)
O6x—K2—P2—O679.81 (6)O4—P2—O6—K1ii148.93 (5)
O6iv—K2—P2—O634.76 (7)K2—P2—O6—K1ii62.82 (7)
O8iv—K2—P2—O64.30 (7)O7—P2—O6—K2iv138.04 (7)
Co1ii—K2—P2—O681.94 (5)O5—P2—O6—K2iv11.82 (8)
P1ii—K2—P2—O639.70 (5)O4—P2—O6—K2iv100.04 (7)
P1ix—K2—P2—O6136.59 (5)K1ii—P2—O6—K2iv111.03 (8)
Co1iv—K2—P2—O638.32 (6)K2—P2—O6—K2iv48.22 (8)
O5vii—K2—P2—O572.37 (7)O6i—Co1—O6—P2166.55 (5)
O2ii—K2—P2—O5123.06 (7)O2—Co1—O6—P215.10 (8)
O2ix—K2—P2—O5172.46 (8)O9—Co1—O6—P275.52 (8)
O8ii—K2—P2—O5178.11 (7)O8—Co1—O6—P2101.36 (8)
O6x—K2—P2—O55.55 (7)K1ii—Co1—O6—P2119.56 (8)
O6iv—K2—P2—O539.50 (7)K2iii—Co1—O6—P254.78 (9)
O8iv—K2—P2—O578.56 (8)K2iv—Co1—O6—P2150.28 (9)
Co1ii—K2—P2—O5156.20 (7)O6i—Co1—O6—K1ii46.99 (5)
P1ii—K2—P2—O5113.97 (7)O2—Co1—O6—K1ii134.65 (3)
P1ix—K2—P2—O5149.14 (7)O9—Co1—O6—K1ii44.03 (4)
Co1iv—K2—P2—O535.95 (7)O8—Co1—O6—K1ii139.08 (4)
O5—K2—P2—O471.56 (8)K2iii—Co1—O6—K1ii174.341 (15)
O5vii—K2—P2—O40.81 (5)K2iv—Co1—O6—K1ii90.17 (3)
O2ii—K2—P2—O4165.38 (5)O6i—Co1—O6—K2iv43.18 (4)
O2ix—K2—P2—O4115.98 (6)O2—Co1—O6—K2iv135.18 (3)
O8ii—K2—P2—O4106.55 (5)O9—Co1—O6—K2iv134.20 (4)
O6x—K2—P2—O466.02 (6)O8—Co1—O6—K2iv48.92 (4)
O6iv—K2—P2—O4111.07 (5)K1ii—Co1—O6—K2iv90.17 (3)
O8iv—K2—P2—O4150.13 (6)K2iii—Co1—O6—K2iv95.49 (3)
Co1ii—K2—P2—O4132.23 (5)O6i—Co1—O8—K2iii135.96 (3)
P1ii—K2—P2—O4174.47 (5)O6—Co1—O8—K2iii135.96 (3)
P1ix—K2—P2—O477.58 (5)O2i—Co1—O8—K2iii43.59 (3)
Co1iv—K2—P2—O4107.51 (5)O2—Co1—O8—K2iii43.59 (3)
O5—K2—P2—K1ii114.55 (7)K1ii—Co1—O8—K2iii180.0
O5vii—K2—P2—K1ii173.07 (3)K2iv—Co1—O8—K2iii180.0
O2ii—K2—P2—K1ii8.50 (2)O6i—Co1—O8—K2iv44.04 (3)
O2ix—K2—P2—K1ii57.90 (4)O6—Co1—O8—K2iv44.04 (3)
O8ii—K2—P2—K1ii67.33 (2)O2i—Co1—O8—K2iv136.41 (3)
O6x—K2—P2—K1ii120.10 (3)O2—Co1—O8—K2iv136.41 (3)
O6iv—K2—P2—K1ii75.05 (2)K1ii—Co1—O8—K2iv0.0
O8iv—K2—P2—K1ii35.99 (4)K2iii—Co1—O8—K2iv180.0
Co1ii—K2—P2—K1ii41.648 (14)O6i—Co1—O9—K1ii44.01 (3)
P1ii—K2—P2—K1ii0.588 (12)O6—Co1—O9—K1ii44.01 (3)
P1ix—K2—P2—K1ii96.30 (2)O2i—Co1—O9—K1ii136.53 (3)
Co1iv—K2—P2—K1ii78.609 (14)O2—Co1—O9—K1ii136.53 (3)
O2—P1—O1—K1133.36 (7)K2iii—Co1—O9—K1ii180.0
O3—P1—O1—K1101.18 (8)K2iv—Co1—O9—K1ii0.0
Symmetry codes: (i) x, y+3/2, z; (ii) x+1/2, y+1, z+1/2; (iii) x+1/2, y+1, z1/2; (iv) x, y+1, z+1; (v) x1/2, y+1/2, z+1/2; (vi) x1/2, y, z+1/2; (vii) x, y+1/2, z; (viii) x+1/2, y1/2, z1/2; (ix) x+1/2, y1/2, z+1/2; (x) x, y1/2, z+1; (xi) x+1/2, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O7xii0.78 (3)1.76 (3)2.5272 (15)170 (4)
O5—H5···O1vi0.76 (3)1.74 (3)2.4996 (15)176 (3)
O8—H8···O2xiii0.81 (3)2.07 (3)2.8255 (17)156 (3)
O9—H9···O7xiv0.85 (3)1.92 (3)2.7669 (14)175 (3)
Symmetry codes: (vi) x1/2, y, z+1/2; (xii) x+1, y+1, z+1; (xiii) x1/2, y+3/2, z+1/2; (xiv) x+1, y+1/2, z+1.

Experimental details

Crystal data
Chemical formula[CoK2(H2P2O7)2]·2H2O
Mr525.07
Crystal system, space groupOrthorhombic, Pnma
Temperature (K)173
a, b, c (Å)9.7044 (5), 11.0023 (6), 13.3937 (8)
V3)1430.05 (14)
Z4
Radiation typeMo Kα
µ (mm1)2.32
Crystal size (mm)0.22 × 0.18 × 0.09
Data collection
DiffractometerSTOE IPDS II two-circle
diffractometer
Absorption correctionMulti-scan
(MULABS; Spek, 1990; Blessing, 1995)
Tmin, Tmax0.630, 0.819
No. of measured, independent and
observed [I > 2σ(I)] reflections
24419, 2441, 2173
Rint0.049
(sin θ/λ)max1)0.732
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.024, 0.061, 1.03
No. of reflections2441
No. of parameters128
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å3)0.37, 0.70

Computer programs: X-AREA (Stoe & Cie, 2001), X-AREA, SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), XP in SHELXTL-Plus (Sheldrick, 1991).

Selected bond lengths (Å) top
Co1—O62.0883 (10)K1—O9iii2.9636 (16)
Co1—O22.0926 (10)K2—O52.7007 (10)
Co1—O92.1018 (14)K2—O2iv2.8149 (10)
Co1—O82.1537 (15)K2—O8iv2.9951 (17)
K1—O3i2.6975 (11)K2—O6v3.0239 (12)
K1—O12.6982 (11)K2—O8vi3.2827 (17)
K1—O6ii2.9621 (10)
Symmetry codes: (i) x1/2, y+1/2, z+1/2; (ii) x+1/2, y1/2, z1/2; (iii) x+1/2, y+1, z1/2; (iv) x+1/2, y+1, z+1/2; (v) x, y1/2, z+1; (vi) x, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3—H3···O7vii0.78 (3)1.76 (3)2.5272 (15)170 (4)
O5—H5···O1viii0.76 (3)1.74 (3)2.4996 (15)176 (3)
O8—H8···O2ix0.81 (3)2.07 (3)2.8255 (17)156 (3)
O9—H9···O7x0.85 (3)1.92 (3)2.7669 (14)175 (3)
Symmetry codes: (vii) x+1, y+1, z+1; (viii) x1/2, y, z+1/2; (ix) x1/2, y+3/2, z+1/2; (x) x+1, y+1/2, z+1.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds