metal-organic papers
m1126
Meng, Zhu, Zeng and Ng [Co(C9H6O5)(H2O)3] doi:10.1107/S1600536805012961 Acta Cryst.(2005). E61, m1126–m1127 Acta Crystallographica Section E
Structure Reports Online
ISSN 1600-5368
mer
-Triaqua(2-carboxylatophenoxyacetato)cobalt(II)
Fa-Yan Meng,aLi-Hong Zhu,b
Ming-Hua Zenga* and
Seik Weng Ngc
aDepartment of Chemistry, Guangxi Normal
University, Guilin 541000, Guangxi, People’s Republic of China,bDepartment of Chemistry,
Huanggang Normal College, Huangzhou 438000, Hubei, People’s Republic of China, andcDepartment of Chemistry, University of Malaya, 50603 Kuala Lumpur, Malaysia
Correspondence e-mail: zmhzsu@163.com
Key indicators
Single-crystal X-ray study
T= 295 K
Mean(C–C) = 0.003 A˚
Rfactor = 0.028
wRfactor = 0.078
Data-to-parameter ratio = 13.6
For details of how these key indicators were automatically derived from the article, see http://journals.iucr.org/e.
#2005 International Union of Crystallography Printed in Great Britain – all rights reserved
In the title compound, [Co(C9H6O5)(H2O)3], the Co II
atom is coordinated by three O atoms from the 2-carboxylato-phenoxyacetate ligand in meridional sites, forming chelate rings. The other three coordination sites of the octahedron are occupied by the water molecules.
Comment
The preceding report describes a polymeric zinc(II) complex with 2-carboxylatophenoxyacetic acid (2-cbphacH2) as a ligand, [Zn(2-cbphac)(H2O)]n; this was synthesized hydro-thermally. The compound adopts a carboxylate-bridged chain motif (Zhuet al., 2005). Under non-hydrothermal conditions, the cobalt(II) compound crystallizes as the title monomeric complex, [Co(2-cbphac)(H2O)3], (I).
In (I), the CoIIatom is coordinated by three O atoms from
the 2-cbphac2 ligand which occupy mer sites; adjacent
complexes are linked by O—H O hydrogen bonds (Table 2) into a three-dimensional network. The cobalt(II) complex of 3-carboxyphenoxyacetic acid (3-cbphacH2) exists as [Co(3-cbphacH)2(H2O)4], in which the 3-carboxyl group retains the acid H atom (Liet al., 2004).
Experimental
Cobalt(II) nitrate hexahydrate (0.149 g, 0.5 mmol) and 2-carboxy-phenoxyacetic acid (0.196 g, 1 mmol) were dissolved in ethanol (3 ml) and water (15 ml) to give a purple solution. Crystals of (I) separated from the solution after a week (yieldca70%).
Crystal data
[Co(C9H6O5)(H2O)3] Mr= 307.12 Monoclinic,P21=c a= 8.762 (1) A˚
b= 6.7707 (8) A˚
c= 19.841 (2) A˚ = 96.515 (2)
V= 1169.5 (2) A˚3 Z= 4
Dx= 1.744 Mg m 3
MoKradiation Cell parameters from 934
reflections = 3.2–27.0 = 1.50 mm1
T= 295 (2) K Block, dark purple 0.360.250.21 mm
Data collection
Bruker SMART 1K area-detector diffractometer
’and!scans
Absorption correction: multi-scan (SADABS; Bruker, 2001)
Tmin= 0.615,Tmax= 0.744
6758 measured reflections
2549 independent reflections 2132 reflections withI> 2(I)
Rint= 0.021 max= 27.0
h=9!11
k=8!7
l=25!22
Refinement
Refinement onF2 R[F2> 2(F2)] = 0.028 wR(F2) = 0.078 S= 1.06 2549 reflections 187 parameters
H atoms treated by a mixture of independent and constrained refinement
w= 1/[2(F
o2) + (0.0461P)2 + 0.1445P]
whereP= (Fo2+ 2Fc2)/3 (/)max= 0.001
max= 0.34 e A˚
3
min=0.20 e A˚
3
Table 1
Selected geometric parameters (A˚ ,).
Co1—O2 2.031 (1)
Co1—O3 2.203 (1)
Co1—O4 1.989 (1)
Co1—O1w 2.097 (2)
Co1—O2w 2.044 (1)
Co1—O3w 2.108 (2)
O2—Co1—O3 76.77 (5)
O2—Co1—O4 160.59 (6)
O2—Co1—O1w 90.82 (7)
O2—Co1—O2w 97.28 (6)
O2—Co1—O3w 89.57 (7)
O3—Co1—O4 83.83 (5)
O3—Co1—O1w 91.69 (6)
O3—Co1—O2w 174.04 (6)
O3—Co1—O3w 90.14 (6)
O4—Co1—O1w 90.28 (7)
O4—Co1—O2w 102.11 (6)
O4—Co1—O3w 89.96 (7)
O1w—Co1—O2w 88.81 (6) O1w—Co1—O3w 178.16 (6) O2w—Co1—O3w 89.35 (6)
O2—C1—C2—O3 0.0 (3)
C2—O3—C3—C4 1.5 (3)
O3—C3—C8—C9 1.7 (3)
C3—C8—C9—O4 3.2 (3)
Table 2
Hydrogen-bonding geometry (A˚ ,).
D—H A D—H H A D A D—H A
O1w—H1w1 O5i
0.85 (1) 1.93 (1) 2.760 (2) 166 (3) O1w—H1w2 O4ii
0.85 (1) 1.97 (1) 2.804 (2) 169 (2) O2w—H2w2 O1iii
0.84 (1) 1.93 (1) 2.766 (2) 173 (2) O2w—H2w1 O5ii 0.84 (1) 1.87 (1) 2.703 (2) 171 (2) O3w—H3w1 O2iii
0.85 (1) 1.92 (1) 2.757 (2) 167 (3) O3w—H3w2 O1iv
0.84 (1) 2.03 (1) 2.861 (2) 172 (2)
Symmetry codes: (i) x;1þy;z; (ii) 2x;1 2þy;
3
2z; (iii) 1x;y 1 2;
3 2z; (iv)
x;y1;z.
The carbon-bound H atoms were positioned geometrically (C—H = 0.93 A˚ for the aromatic H atoms and 0.97 A˚ for the methylene H atoms) and were included in the refinement in the riding-model approximation, withUiso(H) values set at 1.2 timesUeq(C). The water
H atoms were located in difference Fourier maps and refined isotropically, with restraints of O—H and H H distances to 0.85 (1) and 1.39 (1) A˚ , respectively.
Data collection:SMART(Bruker, 2001); cell refinement:SAINT (Bruker, 2001); data reduction:SAINT; 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.
We thank the Guangxi Normal University and the Univer-sity of Malaya for supporting this study.
References
Bruker (2001).SADABS(Version 6.45),SAINT(Version 6.45) andSMART
(Version 5.0). Bruker AXS Inc, Madison, Wisconsin, USA.
Johnson, C. K. (1976).ORTEPII. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA.
Li, S.-J., Gu, C.-S., Gao, S., Zhao, H., Zhao, J.-G. & Huo, L.-H. (2004).Chin. J. Struct. Chem.23, 835–838.
Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Go¨ttingen, Germany.
[image:2.610.317.563.70.333.2]Zhu, L.-H., Zeng, M.-H. & Ng, S. W. (2005).Acta Cryst.E61, m916–m918. Figure 1
supporting information
sup-1 Acta Cryst. (2005). E61, m1126–m1127
supporting information
Acta Cryst. (2005). E61, m1126–m1127 [https://doi.org/10.1107/S1600536805012961]
mer
-Triaqua(2-carboxylatophenoxyacetato)cobalt(II)
Fa-Yan Meng, Li-Hong Zhu, Ming-Hua Zeng and Seik Weng Ng
Triaqua(2-carboxylatophenoxyactetato)cobalt(II)
Crystal data
[Co(C9H6O5)(H2O)3]
Mr = 307.12
Monoclinic, P21/c
Hall symbol: -P 2ybc a = 8.762 (1) Å b = 6.7707 (8) Å c = 19.841 (2) Å β = 96.515 (2)° V = 1169.5 (2) Å3
Z = 4
F(000) = 628 Dx = 1.744 Mg m−3
Mo Kα radiation, λ = 0.71073 Å Cell parameters from 934 reflections θ = 3.2–27.0°
µ = 1.50 mm−1
T = 295 K
Block, dark purple 0.36 × 0.25 × 0.21 mm
Data collection
Bruker SMART 1K area-detector diffractometer
Radiation source: medium-focus sealed tube Graphite monochromator
φ and ω scans
Absorption correction: multi-scan (SADABS; Bruker, 2002) Tmin = 0.615, Tmax = 0.744
6758 measured reflections 2549 independent reflections 2132 reflections with I > 2σ(I) Rint = 0.021
θmax = 27.0°, θmin = 2.1°
h = −9→11 k = −8→7 l = −25→22
Refinement
Refinement on F2
Least-squares matrix: full R[F2 > 2σ(F2)] = 0.028
wR(F2) = 0.078
S = 1.06 2549 reflections 187 parameters 9 restraints
Primary atom site location: structure-invariant direct methods
Secondary atom site location: difference Fourier map
Hydrogen site location: inferred from neighbouring sites
H atoms treated by a mixture of independent and constrained refinement
w = 1/[σ2(F
o2) + (0.0461P)2 + 0.1445P]
where P = (Fo2 + 2Fc2)/3
(Δ/σ)max = 0.001
Δρmax = 0.34 e Å−3
Δρmin = −0.20 e Å−3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2)
x y z Uiso*/Ueq
O2 0.6033 (2) 0.8508 (2) 0.6891 (1) 0.0381 (4) O3 0.6994 (2) 0.6452 (2) 0.5895 (1) 0.0311 (3) O4 0.8605 (2) 0.3735 (2) 0.6775 (1) 0.0409 (4) O5 0.9543 (2) 0.1180 (2) 0.6288 (1) 0.0392 (4) O1w 0.9369 (2) 0.7831 (2) 0.7069 (1) 0.0421 (4) O2w 0.7601 (2) 0.5956 (3) 0.8040 (1) 0.0403 (4) O3w 0.5409 (2) 0.4289 (2) 0.6973 (1) 0.0405 (4) C1 0.5630 (2) 0.9216 (3) 0.6317 (1) 0.0295 (4) C2 0.6106 (2) 0.8179 (3) 0.5695 (1) 0.0319 (4) C3 0.7462 (2) 0.5282 (3) 0.5380 (1) 0.0258 (4) C4 0.7105 (3) 0.5811 (3) 0.4706 (1) 0.0372 (5) C5 0.7591 (3) 0.4665 (4) 0.4193 (1) 0.0442 (6) C6 0.8419 (3) 0.2977 (4) 0.4345 (1) 0.0472 (6) C7 0.8755 (2) 0.2443 (3) 0.5016 (1) 0.0396 (5) C8 0.8306 (2) 0.3559 (3) 0.5551 (1) 0.0274 (4) C9 0.8836 (2) 0.2790 (3) 0.6250 (1) 0.0285 (4) H1w1 0.930 (3) 0.894 (2) 0.687 (1) 0.054 (8)* H1w2 0.992 (3) 0.798 (4) 0.744 (1) 0.071 (9)* H2w1 0.845 (1) 0.613 (3) 0.827 (1) 0.037 (6)* H2w2 0.689 (2) 0.581 (4) 0.829 (1) 0.052 (8)* H3w1 0.508 (3) 0.415 (3) 0.736 (1) 0.063 (9)* H3w2 0.533 (3) 0.320 (2) 0.677 (1) 0.054 (8)*
H2a 0.5199 0.7804 0.5396 0.038*
H2b 0.6710 0.9071 0.5449 0.038*
H4 0.6534 0.6948 0.4597 0.045*
H5 0.7353 0.5045 0.3743 0.053*
H6 0.8748 0.2204 0.4002 0.057*
H7 0.9307 0.1287 0.5117 0.048*
Atomic displacement parameters (Å2)
U11 U22 U33 U12 U13 U23
supporting information
sup-3 Acta Cryst. (2005). E61, m1126–m1127
C8 0.026 (1) 0.025 (1) 0.030 (1) 0.002 (1) 0.002 (1) −0.001 (1) C9 0.026 (1) 0.025 (1) 0.034 (1) 0.003 (1) 0.001 (1) 0.000 (1)
Geometric parameters (Å, º)
Co1—O2 2.031 (1) O3w—H3w1 0.85 (1)
Co1—O3 2.203 (1) O3w—H3w2 0.84 (1)
Co1—O4 1.989 (1) C1—C2 1.520 (3)
Co1—O1w 2.097 (2) C3—C4 1.385 (3)
Co1—O2w 2.044 (1) C3—C8 1.403 (3)
Co1—O3w 2.108 (2) C4—C5 1.385 (3)
O1—C1 1.244 (2) C5—C6 1.369 (3)
O2—C1 1.249 (2) C6—C7 1.379 (3)
O3—C3 1.392 (2) C7—C8 1.395 (3)
O3—C2 1.436 (2) C8—C9 1.504 (3)
O4—C9 1.259 (2) C2—H2a 0.97
O5—C9 1.252 (2) C2—H2b 0.97
O1w—H1w1 0.85 (1) C4—H4 0.93
O1w—H1w2 0.85 (1) C5—H5 0.93
O2w—H2w1 0.84 (1) C6—H6 0.93
O2w—H2w2 0.84 (1) C7—H7 0.93
O2—Co1—O3 76.77 (5) C6—C7—C8 123.0 (2)
O2—Co1—O4 160.59 (6) C7—C8—C3 116.9 (2)
O2—Co1—O1w 90.82 (7) C7—C8—C9 115.4 (2)
O2—Co1—O2w 97.28 (6) C3—C8—C9 127.6 (2)
O2—Co1—O3w 89.57 (7) O5—C9—O4 121.1 (2)
O3—Co1—O4 83.83 (5) O5—C9—C8 117.2 (2)
O3—Co1—O1w 91.69 (6) O4—C9—C8 121.7 (2)
O3—Co1—O2w 174.04 (6) Co1—O1w—H1w1 117 (2)
O3—Co1—O3w 90.14 (6) Co1—O1w—H1w2 121 (2)
O4—Co1—O1w 90.28 (7) H1w1—O1w—H1w2 108 (2)
O4—Co1—O2w 102.11 (6) Co1—O2w—H2w1 121 (1)
O4—Co1—O3w 89.96 (7) Co1—O2w—H2w2 127 (1)
O1w—Co1—O2w 88.81 (6) H2w1—O2w—H2w2 112 (2)
O1w—Co1—O3w 178.16 (6) Co1—O3w—H3w1 114 (2)
O2w—Co1—O3w 89.35 (6) Co1—O3w—H3w2 122 (2)
C1—O2—Co1 120.9 (1) H3w1—O3w—H3w2 109 (2)
C3—O3—C2 117.1 (1) O3—C2—H2a 109.7
C3—O3—Co1 129.9 (1) C1—C2—H2a 109.7
C2—O3—Co1 113.0 (1) O3—C2—H2b 109.7
C9—O4—Co1 137.3 (1) C1—C2—H2b 109.7
O1—C1—O2 125.5 (2) H2a—C2—H2b 108.2
O1—C1—C2 115.3 (2) C3—C4—H4 119.7
O2—C1—C2 119.3 (2) C5—C4—H4 119.7
O3—C2—C1 109.9 (2) C6—C5—H5 119.8
C4—C3—O3 120.6 (2) C4—C5—H5 119.8
O3—C3—C8 119.1 (2) C7—C6—H6 120.6
C3—C4—C5 120.7 (2) C6—C7—H7 118.5
C6—C5—C4 120.3 (2) C8—C7—H7 118.5
C5—C6—C7 118.8 (2)
O4—Co1—O2—C1 −4.7 (3) O2—C1—C2—O3 0.0 (3)
O2w—Co1—O2—C1 177.4 (2) C2—O3—C3—C4 1.5 (3)
O1w—Co1—O2—C1 88.4 (2) Co1—O3—C3—C4 −179.1 (1)
O3w—Co1—O2—C1 −93.4 (2) C2—O3—C3—C8 −178.8 (2)
O3—Co1—O2—C1 −3.1 (2) Co1—O3—C3—C8 0.7 (3)
O4—Co1—O3—C3 2.9 (2) O3—C3—C4—C5 179.0 (2)
O2—Co1—O3—C3 −176.6 (2) C8—C3—C4—C5 −0.8 (3)
O1w—Co1—O3—C3 93.0 (2) C3—C4—C5—C6 0.7 (4)
O3w—Co1—O3—C3 −87.1 (2) C4—C5—C6—C7 0.1 (4)
O4—Co1—O3—C2 −177.7 (1) C5—C6—C7—C8 −0.8 (4)
O2—Co1—O3—C2 2.9 (1) C6—C7—C8—C3 0.7 (3)
O1w—Co1—O3—C2 −87.6 (1) C6—C7—C8—C9 −177.5 (2)
O3w—Co1—O3—C2 92.4 (1) C4—C3—C8—C7 0.1 (3)
O2—Co1—O4—C9 −7.5 (4) O3—C3—C8—C7 −179.6 (2)
O2w—Co1—O4—C9 170.4 (2) C4—C3—C8—C9 178.0 (2)
O1w—Co1—O4—C9 −100.8 (2) O3—C3—C8—C9 −1.7 (3)
O3w—Co1—O4—C9 81.1 (2) Co1—O4—C9—O5 −170.6 (2)
O3—Co1—O4—C9 −9.1 (2) Co1—O4—C9—C8 10.6 (3)
Co1—O2—C1—O1 −177.1 (2) C7—C8—C9—O5 −4.1 (3)
Co1—O2—C1—C2 2.7 (3) C3—C8—C9—O5 178.0 (2)
C3—O3—C2—C1 177.2 (2) C7—C8—C9—O4 174.7 (2)
Co1—O3—C2—C1 −2.4 (2) C3—C8—C9—O4 −3.2 (3)
O1—C1—C2—O3 179.9 (2)
Hydrogen-bond geometry (Å, º)
D—H···A D—H H···A D···A D—H···A
O1w—H1w1···O5i 0.85 (1) 1.93 (1) 2.760 (2) 166 (3)
O1w—H1w2···O4ii 0.85 (1) 1.97 (1) 2.804 (2) 169 (2)
O2w—H2w2···O1iii 0.84 (1) 1.93 (1) 2.766 (2) 173 (2)
O2w—H2w1···O5ii 0.84 (1) 1.87 (1) 2.703 (2) 171 (2)
O3w—H3w1···O2iii 0.85 (1) 1.92 (1) 2.757 (2) 167 (3)
O3w—H3w2···O1iv 0.84 (1) 2.03 (1) 2.861 (2) 172 (2)
