Buy article online - an online subscription or single-article purchase is required to access this article.
In the title compound, [Co2(C10H8O5)2(H2O)8]·4H2O, two tetraaquacobalt(II) cations are bridged by two 3-(4-carboxylatophenoxy)propionate dianions across a center of inversion, giving rise to a dinuclear molecule; the coordinating O atoms that comprise the octahedral coordination polyhedron around the metal are cis to each other. Hydrogen bonds link the dinuclear molecules into a three-dimensional network. The disordered uncoordinated water molecules occupy cavities within the framework.
Supporting information
CCDC reference: 621345
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.006 Å
- H-atom completeness 81%
- Disorder in solvent or counterion
- R factor = 0.047
- wR factor = 0.173
- Data-to-parameter ratio = 16.5
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT430_ALERT_2_A Short Inter D...A Contact O5W' .. O5W .. 1.93 Ang.
| Author Response: Two water molecules are disordered over three positions. The
three positions are refined with 2/3 occupancies. Hydrogen atoms were not
added.
|
PLAT430_ALERT_2_A Short Inter D...A Contact O5W' .. O5W" .. 1.95 Ang.
| Author Response: Two water molecules are disordered over three positions. The
three positions are refined with 2/3 occupancies. Hydrogen atoms were not
added.
|
PLAT430_ALERT_2_A Short Inter D...A Contact O5W" .. O5W .. 2.16 Ang.
| Author Response: Two water molecules are disordered over three positions. The
three positions are refined with 2/3 occupancies. Hydrogen atoms were not
added.
|
Alert level B
PLAT430_ALERT_2_B Short Inter D...A Contact O5W' .. O5W" .. 2.84 Ang.
| Author Response: Two water molecules are disordered over three positions. The
three positions are refined with 2/3 occupancies. Hydrogen atoms were not
added.
|
PLAT430_ALERT_2_B Short Inter D...A Contact O5W' .. O5W .. 2.84 Ang.
| Author Response: Two water molecules are disordered over three positions. The
three positions are refined with 2/3 occupancies. Hydrogen atoms were not
added.
|
PLAT430_ALERT_2_B Short Inter D...A Contact O5W" .. O5W .. 2.84 Ang.
| Author Response: Two water molecules are disordered over three positions. The
three positions are refined with 2/3 occupancies. Hydrogen atoms were not
added.
|
Alert level C
CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
the range 0.99 <> 1.01
From the CIF: _cell_formula_units_Z 2
From the CIF: _chemical_formula_weight 750.38
TEST: Calculate formula weight from _atom_site_*
atom mass num sum
C 12.01 20.00 240.22
H 1.01 32.00 32.26
O 16.00 22.02 352.30
Co 58.93 2.00 117.87
Calculated formula weight 742.64
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 750.38
PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 1.01
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Co1
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.46
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 67.00 Perc.
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O5W"
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O5W
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10
Alert level G
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:C20 H40 Co2 O22
Atom count from the _atom_site data: C20 H32 Co2 O22.02
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 2
From the CIF: _chemical_formula_sum C20 H40 Co2 O22
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 40.00 40.00 0.00
H 80.00 64.00 16.00
Co 4.00 4.00 0.00
O 44.00 44.04 -0.04
3 ALERT level A = In general: serious problem
3 ALERT level B = Potentially serious problem
15 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
13 ALERT type 2 Indicator that the structure model may be wrong or deficient
0 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: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Bis[µ-3-(4-carboxylatophenoxy)propionato-
κ2O:
O']bis[tetraaquacobalt(II)] tetrahydrate
top
Crystal data top
[Co2(C10H8O5)2(H2O)8]·4H2O | F(000) = 780 |
Mr = 750.38 | Dx = 1.669 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 9413 reflections |
a = 18.277 (4) Å | θ = 3.0–27.5° |
b = 7.281 (2) Å | µ = 1.20 mm−1 |
c = 11.303 (2) Å | T = 295 K |
β = 96.84 (2)° | Block, pink |
V = 1493.4 (5) Å3 | 0.37 × 0.29 × 0.18 mm |
Z = 2 | |
Data collection top
Rigaku RAXIS-RAPID IP diffractometer | 3422 independent reflections |
Radiation source: fine-focus sealed tube | 2336 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.036 |
ω scans | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −23→23 |
Tmin = 0.651, Tmax = 0.795 | k = −9→8 |
14137 measured reflections | l = −14→14 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.047 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.173 | H-atom parameters constrained |
S = 1.15 | w = 1/[σ2(Fo2) + (0.0674P)2 + 4.709P] where P = (Fo2 + 2Fc2)/3 |
3422 reflections | (Δ/σ)max = 0.001 |
208 parameters | Δρmax = 0.47 e Å−3 |
0 restraints | Δρmin = −1.00 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Co1 | 0.66907 (3) | 0.49806 (8) | 0.49571 (4) | 0.0197 (2) | |
O1 | 0.7526 (2) | 0.4835 (6) | 0.3941 (3) | 0.043 (1) | |
O2 | 0.7077 (2) | 0.4903 (5) | 0.2018 (3) | 0.031 (1) | |
O3 | 1.0504 (2) | 0.4322 (6) | 0.1632 (3) | 0.042 (1) | |
O4 | 1.3097 (2) | 0.4906 (5) | 0.1958 (3) | 0.032 (1) | |
O5 | 1.2525 (2) | 0.4972 (6) | 0.3581 (3) | 0.040 (1) | |
O1w | 0.6603 (2) | 0.2111 (5) | 0.4987 (3) | 0.036 (1) | |
O2w | 0.5859 (2) | 0.5004 (5) | 0.6113 (3) | 0.032 (1) | |
O3w | 0.6657 (2) | 0.7844 (5) | 0.4981 (3) | 0.041 (1) | |
O4w | 0.5952 (2) | 0.5025 (5) | 0.3338 (3) | 0.034 (1) | |
O5w | 0.5009 (4) | 0.805 (1) | 0.6615 (6) | 0.062 (2) | 0.67 |
O5w' | 0.5015 (4) | 0.896 (1) | 0.5008 (9) | 0.088 (3) | 0.67 |
O5w" | 0.4985 (4) | 0.805 (1) | 0.3385 (6) | 0.063 (2) | 0.67 |
C1 | 0.7609 (2) | 0.4789 (6) | 0.2848 (4) | 0.025 (1) | |
C2 | 0.8378 (2) | 0.4611 (6) | 0.2551 (4) | 0.025 (1) | |
C3 | 0.8525 (2) | 0.4495 (8) | 0.1381 (4) | 0.036 (1) | |
C4 | 0.9235 (3) | 0.4373 (9) | 0.1101 (4) | 0.044 (1) | |
C5 | 0.9823 (2) | 0.4391 (8) | 0.2009 (4) | 0.033 (1) | |
C6 | 0.9689 (3) | 0.4461 (8) | 0.3193 (4) | 0.039 (1) | |
C7 | 0.8966 (3) | 0.4583 (7) | 0.3447 (4) | 0.035 (1) | |
C8 | 1.1142 (2) | 0.4518 (7) | 0.2493 (4) | 0.032 (1) | |
C9 | 1.1782 (2) | 0.4652 (7) | 0.1755 (4) | 0.029 (1) | |
C10 | 1.2523 (2) | 0.4853 (6) | 0.2488 (4) | 0.025 (1) | |
H1w1 | 0.6786 | 0.1659 | 0.4394 | 0.053* | |
H1w2 | 0.6836 | 0.1698 | 0.5629 | 0.053* | |
H2w1 | 0.5601 | 0.5972 | 0.5993 | 0.048* | |
H2w2 | 0.6058 | 0.4982 | 0.6832 | 0.048* | |
H3w1 | 0.6911 | 0.8239 | 0.5609 | 0.061* | |
H3w2 | 0.6833 | 0.8264 | 0.4372 | 0.061* | |
H4w1 | 0.6198 | 0.5073 | 0.2747 | 0.051* | |
H4w2 | 0.5690 | 0.4058 | 0.3292 | 0.051* | |
H3 | 0.8135 | 0.4501 | 0.0771 | 0.044* | |
H4 | 0.9324 | 0.4278 | 0.0310 | 0.052* | |
H6 | 1.0078 | 0.4426 | 0.3804 | 0.047* | |
H7 | 0.8874 | 0.4648 | 0.4237 | 0.042* | |
H8a | 1.1198 | 0.3463 | 0.3020 | 0.039* | |
H8b | 1.1107 | 0.5618 | 0.2967 | 0.039* | |
H9a | 1.1788 | 0.3558 | 0.1267 | 0.035* | |
H9b | 1.1703 | 0.5698 | 0.1224 | 0.035* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0191 (3) | 0.0234 (3) | 0.0167 (3) | 0.0000 (2) | 0.0026 (2) | −0.0002 (2) |
O1 | 0.024 (2) | 0.085 (3) | 0.020 (2) | 0.000 (2) | 0.006 (1) | 0.000 (2) |
O2 | 0.024 (1) | 0.048 (2) | 0.022 (1) | 0.002 (2) | 0.004 (1) | 0.001 (2) |
O3 | 0.020 (2) | 0.084 (3) | 0.023 (2) | −0.004 (2) | 0.004 (1) | −0.006 (2) |
O4 | 0.024 (1) | 0.052 (2) | 0.022 (2) | 0.000 (2) | 0.005 (1) | −0.003 (2) |
O5 | 0.025 (2) | 0.076 (3) | 0.018 (1) | 0.000 (2) | 0.000 (1) | −0.004 (2) |
O1w | 0.051 (2) | 0.029 (2) | 0.027 (2) | 0.008 (2) | 0.005 (2) | 0.000 (1) |
O2w | 0.026 (2) | 0.045 (2) | 0.027 (2) | 0.003 (2) | 0.007 (1) | 0.000 (2) |
O3w | 0.068 (3) | 0.027 (2) | 0.028 (2) | −0.010 (2) | 0.010 (2) | 0.000 (1) |
O4w | 0.024 (1) | 0.052 (2) | 0.026 (2) | −0.002 (2) | 0.004 (1) | 0.000 (2) |
O5w | 0.057 (4) | 0.065 (4) | 0.064 (5) | −0.003 (3) | 0.006 (3) | −0.007 (4) |
O5w' | 0.071 (5) | 0.072 (5) | 0.117 (7) | −0.001 (4) | −0.006 (5) | 0.003 (5) |
O5w" | 0.065 (4) | 0.061 (4) | 0.062 (5) | 0.010 (3) | 0.005 (3) | 0.006 (3) |
C1 | 0.024 (2) | 0.030 (2) | 0.021 (2) | −0.002 (2) | 0.006 (2) | 0.000 (2) |
C2 | 0.021 (2) | 0.034 (3) | 0.021 (2) | −0.001 (2) | 0.004 (2) | −0.002 (2) |
C3 | 0.020 (2) | 0.069 (4) | 0.020 (2) | −0.001 (2) | 0.001 (2) | 0.003 (2) |
C4 | 0.025 (2) | 0.087 (4) | 0.018 (2) | −0.008 (2) | 0.005 (2) | −0.006 (2) |
C5 | 0.021 (2) | 0.053 (3) | 0.026 (2) | −0.003 (2) | 0.006 (2) | −0.002 (2) |
C6 | 0.023 (2) | 0.073 (4) | 0.021 (2) | −0.002 (2) | 0.000 (2) | 0.002 (2) |
C7 | 0.027 (2) | 0.058 (3) | 0.021 (2) | 0.000 (2) | 0.005 (2) | 0.000 (2) |
C8 | 0.023 (2) | 0.052 (3) | 0.023 (2) | 0.000 (2) | 0.002 (2) | −0.001 (2) |
C9 | 0.022 (2) | 0.047 (3) | 0.019 (2) | −0.003 (2) | 0.002 (2) | −0.003 (2) |
C10 | 0.025 (2) | 0.030 (2) | 0.020 (2) | 0.001 (2) | 0.006 (2) | 0.001 (2) |
Geometric parameters (Å, º) top
Co1—O1 | 2.020 (3) | C8—C9 | 1.519 (6) |
Co1—O5i | 2.055 (3) | C9—C10 | 1.508 (6) |
Co1—O1w | 2.096 (3) | O1w—H1w1 | 0.85 |
Co1—O2w | 2.119 (3) | O1w—H1w2 | 0.85 |
Co1—O3w | 2.086 (4) | O2w—H2w1 | 0.85 |
Co1—O4w | 2.141 (3) | O2w—H2w2 | 0.85 |
O1—C1 | 1.263 (5) | O3w—H3w1 | 0.85 |
O2—C1 | 1.271 (5) | O3w—H3w2 | 0.85 |
O3—C5 | 1.364 (5) | O4w—H4w1 | 0.85 |
O3—C8 | 1.435 (5) | O4w—H4w2 | 0.85 |
O4—C10 | 1.269 (5) | C3—H3 | 0.93 |
O5—C10 | 1.238 (5) | C4—H4 | 0.93 |
C1—C2 | 1.488 (6) | C6—H6 | 0.93 |
C2—C3 | 1.383 (6) | C7—H7 | 0.93 |
C2—C7 | 1.387 (6) | C8—H8a | 0.97 |
C3—C4 | 1.376 (6) | C8—H8b | 0.97 |
C4—C5 | 1.394 (6) | C9—H9a | 0.97 |
C5—C6 | 1.390 (6) | C9—H9b | 0.97 |
C6—C7 | 1.388 (6) | | |
| | | |
O1—Co1—O5i | 87.5 (1) | O5—C10—O4 | 124.4 (4) |
O1—Co1—O1w | 91.2 (2) | O5—C10—C9 | 116.7 (4) |
O1—Co1—O2w | 175.8 (1) | O4—C10—C9 | 118.9 (4) |
O1—Co1—O3w | 94.9 (2) | Co1—O1w—H1w1 | 109.6 |
O1—Co1—O4w | 87.6 (1) | Co1—O1w—H1w2 | 109.5 |
O5i—Co1—O1w | 92.9 (2) | H1w1—O1w—H1w2 | 109.4 |
O5i—Co1—O2w | 89.3 (1) | Co1—O2w—H2w1 | 109.5 |
O5i—Co1—O3w | 89.5 (2) | Co1—O2w—H2w2 | 109.4 |
O5i—Co1—O4w | 174.6 (1) | H2w1—O2w—H2w2 | 109.5 |
O1w—Co1—O2w | 86.3 (1) | Co1—O3w—H3w1 | 109.6 |
O1w—Co1—O3w | 173.5 (1) | Co1—O3w—H3w2 | 109.6 |
O1w—Co1—O4w | 89.3 (1) | H3w1—O3w—H3w2 | 109.4 |
O2w—Co1—O3w | 87.7 (1) | Co1—O4w—H4w1 | 109.5 |
O2w—Co1—O4w | 95.8 (1) | Co1—O4w—H4w2 | 109.5 |
O3w—Co1—O4w | 88.8 (1) | H4w1—O4w—H4w2 | 109.5 |
C1—O1—Co1 | 138.1 (3) | C4—C3—H3 | 119.4 |
C5—O3—C8 | 118.9 (4) | C2—C3—H3 | 119.4 |
C10—O5—Co1i | 136.3 (3) | C3—C4—H4 | 120.1 |
O1—C1—O2 | 123.3 (4) | C5—C4—H4 | 120.1 |
O1—C1—C2 | 116.7 (4) | C7—C6—H6 | 120.6 |
O2—C1—C2 | 119.9 (4) | C5—C6—H6 | 120.6 |
C3—C2—C7 | 118.4 (4) | C6—C7—H7 | 119.2 |
C3—C2—C1 | 121.1 (4) | C2—C7—H7 | 119.2 |
C7—C2—C1 | 120.5 (4) | O3—C8—H8a | 110.8 |
C4—C3—C2 | 121.3 (4) | C9—C8—H8a | 110.8 |
C3—C4—C5 | 119.7 (4) | O3—C8—H8b | 110.8 |
O3—C5—C6 | 125.0 (4) | C9—C8—H8b | 110.8 |
O3—C5—C4 | 114.9 (4) | H8a—C8—H8b | 108.9 |
C6—C5—C4 | 120.1 (4) | C10—C9—H9a | 108.8 |
C7—C6—C5 | 118.8 (4) | C8—C9—H9a | 108.8 |
C6—C7—C2 | 121.7 (4) | C10—C9—H9b | 108.8 |
O3—C8—C9 | 104.5 (3) | C8—C9—H9b | 108.8 |
C10—C9—C8 | 113.9 (4) | H9a—C9—H9b | 107.7 |
| | | |
O5i—Co1—O1—C1 | −177.8 (5) | C8—O3—C5—C4 | 173.9 (5) |
O3w—Co1—O1—C1 | −88.5 (5) | C3—C4—C5—O3 | −178.0 (6) |
O1w—Co1—O1—C1 | 89.3 (5) | C3—C4—C5—C6 | 2.5 (9) |
O4w—Co1—O1—C1 | 0.1 (5) | O3—C5—C6—C7 | 178.1 (5) |
Co1—O1—C1—O2 | 2.7 (8) | C4—C5—C6—C7 | −2.5 (9) |
Co1—O1—C1—C2 | −177.9 (4) | C5—C6—C7—C2 | 0.9 (9) |
O1—C1—C2—C3 | 178.1 (5) | C3—C2—C7—C6 | 0.6 (8) |
O2—C1—C2—C3 | −2.5 (7) | C1—C2—C7—C6 | −178.5 (5) |
O1—C1—C2—C7 | −2.8 (7) | C5—O3—C8—C9 | −172.1 (5) |
O2—C1—C2—C7 | 176.6 (4) | O3—C8—C9—C10 | −179.5 (4) |
C7—C2—C3—C4 | −0.6 (8) | Co1i—O5—C10—O4 | −7.7 (8) |
C1—C2—C3—C4 | 178.5 (5) | Co1i—O5—C10—C9 | 173.0 (3) |
C2—C3—C4—C5 | −1.0 (9) | C8—C9—C10—O5 | −3.2 (6) |
C8—O3—C5—C6 | −6.6 (8) | C8—C9—C10—O4 | 177.4 (4) |
Symmetry code: (i) −x+2, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O4ii | 0.85 | 2.02 | 2.828 (5) | 158 |
O1w—H1w2···O2iii | 0.85 | 1.96 | 2.774 (5) | 159 |
O2w—H2w1···O5w | 0.85 | 2.03 | 2.804 (8) | 150 |
O2w—H2w2···O4i | 0.85 | 1.94 | 2.722 (4) | 153 |
O3w—H3w1···O2iv | 0.85 | 2.09 | 2.858 (5) | 151 |
O3w—H3w2···O4v | 0.85 | 1.94 | 2.737 (5) | 156 |
O4w—H4w1···O2 | 0.85 | 1.89 | 2.682 (4) | 154 |
O4w—H4w2···O5wvi | 0.85 | 2.01 | 2.850 (8) | 171 |
Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x+2, y−1/2, −z+1/2; (iii) x, −y+1/2, z+1/2; (iv) x, −y+3/2, z+1/2; (v) −x+2, y+1/2, −z+1/2; (vi) −x+1, −y+1, −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.