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In the title compound, [Co(H
2O)
6](C
6H
4NO
3)
2, the Co
II atom lies on a special position of 2/
m site symmetry in an octahedron made up of water molecules. The anions show orientational disorder over mirror planes and are linked together by a pair of N—H
O hydrogen bonds into a dianion. The complex cations and dianions are connected through O—H
O hydrogen bonds to form a three-dimensional network.
Supporting information
CCDC reference: 274604
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (o-O) = 0.004 Å
- Disorder in main residue
- R factor = 0.054
- wR factor = 0.159
- Data-to-parameter ratio = 8.6
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.93
| Author Response: The fraction is low at 55\% but is 96% at 50\%.
|
Alert level B
ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75
Tmin and Tmax reported: 0.499 0.920
Tmin' and Tmax expected: 0.692 0.918
RR' = 0.720
Please check that your absorption correction is appropriate.
PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.71
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Co1
PLAT301_ALERT_3_B Main Residue Disorder ......................... 29.00 Perc.
PLAT731_ALERT_1_B Bond Calc 0.85(5), Rep 0.850(10) ...... 5.00 su-Rat
O2W -H2W2 1.555 1.555
PLAT735_ALERT_1_B D-H Calc 0.85(5), Rep 0.850(10) ...... 5.00 su-Rat
O2W -H4# 1.555 1.555
PLAT735_ALERT_1_B D-H Calc 0.85(5), Rep 0.850(10) ...... 5.00 su-Rat
O2W -H4# 1.555 1.555
Alert level C
REFLT03_ALERT_3_C Reflection count < 95% complete
From the CIF: _diffrn_reflns_theta_max 27.40
From the CIF: _diffrn_reflns_theta_full 27.40
From the CIF: _reflns_number_total 968
TEST2: Reflns within _diffrn_reflns_theta_max
Count of symmetry unique reflns 1041
Completeness (_total/calc) 92.99%
PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.93
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 8.57
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.05
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat
O1W -H1W2 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat
O2W -H2W1 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 110(5), Rep 110(2) ...... 2.50 su-Rat
H2W1 -O2W -H2W2 1.555 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat
O1W -H2# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat
O2W -H3# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Rat
O2W -H3# 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.87(3), Rep 1.870(10) ...... 3.00 su-Rat
H2# -O1 1.555 7.666
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.13 Ratio
1 ALERT level A = In general: serious problem
7 ALERT level B = Potentially serious problem
17 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
14 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 ALERT type 2 Indicator that the structure model may be wrong or deficient
7 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: atomic coordinates taken from the isostructural Zn analogue (Zhang et al.,
2005); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Hexaaquacobalt(II) bis(6-hydroxypyridine-3-carboxylate)
top
Crystal data top
[Co(H2O)6](C6H4NO3)2 | F(000) = 458 |
Mr = 443.23 | Dx = 1.707 Mg m−3 |
Monoclinic, C2/m | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1422 reflections |
a = 11.609 (1) Å | θ = 2.7–27.4° |
b = 9.754 (1) Å | µ = 1.07 mm−1 |
c = 7.6157 (8) Å | T = 295 K |
β = 91.448 (2)° | Plate, red |
V = 862.1 (2) Å3 | 0.34 × 0.20 × 0.08 mm |
Z = 2 | |
Data collection top
Bruker APEX area-detector diffractometer | 968 independent reflections |
Radiation source: fine-focus sealed tube | 956 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
φ and ω scans | θmax = 27.4°, θmin = 2.7° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −14→15 |
Tmin = 0.499, Tmax = 0.920 | k = −12→12 |
2296 measured reflections | l = −9→8 |
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)] = 0.054 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.159 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.19 | w = 1/[σ2(Fo2) + (0.053P)2 + 7.1943P] where P = (Fo2 + 2Fc2)/3 |
968 reflections | (Δ/σ)max = 0.001 |
113 parameters | Δρmax = 0.54 e Å−3 |
14 restraints | Δρmin = −0.50 e Å−3 |
Special details top
Refinement. A dimensionless value, 2µ*r (r = equivalent radius of crystal) of 0.23, was
used in the absorption correction step. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Co1 | 0.5000 | 0.5000 | 0.5000 | 0.0214 (3) | |
O1 | 0.8314 (3) | 0.6134 (4) | 0.6609 (5) | 0.048 (1) | |
O2 | 1.3222 (5) | 0.5756 (7) | 0.9709 (9) | 0.038 (2) | 0.50 |
O1W | 0.6265 (3) | 0.6455 (4) | 0.5021 (6) | 0.055 (1) | |
O2W | 0.4893 (5) | 0.5000 | 0.2226 (7) | 0.065 (2) | |
N1 | 1.1453 (5) | 0.6558 (8) | 0.888 (1) | 0.035 (2) | 0.50 |
C1 | 1.0373 (7) | 0.640 (1) | 0.8183 (9) | 0.030 (2) | 0.50 |
C2 | 0.9997 (6) | 0.513 (1) | 0.7604 (9) | 0.030 (2) | 0.50 |
C3 | 1.0756 (7) | 0.404 (1) | 0.776 (1) | 0.033 (2) | 0.50 |
C4 | 1.1858 (7) | 0.420 (1) | 0.847 (1) | 0.034 (2) | 0.50 |
C5 | 1.2225 (8) | 0.5505 (9) | 0.904 (1) | 0.030 (2) | 0.50 |
C6 | 0.8778 (5) | 0.5000 | 0.6882 (8) | 0.029 (1) | |
H2O | 1.3299 | 0.6615 | 0.9859 | 0.045* | 0.50 |
H1W1 | 0.688 (2) | 0.625 (4) | 0.559 (5) | 0.03 (1)* | |
H1W2 | 0.632 (4) | 0.723 (3) | 0.454 (6) | 0.04 (2)* | |
H2W1 | 0.426 (3) | 0.5000 | 0.164 (8) | 0.04 (2)* | |
H2W2 | 0.545 (4) | 0.5000 | 0.153 (7) | 0.08 (3)* | |
H1 | 0.9882 | 0.7152 | 0.8096 | 0.037* | 0.50 |
H3 | 1.0519 | 0.3180 | 0.7379 | 0.040* | 0.50 |
H4 | 1.2352 | 0.3451 | 0.8563 | 0.041* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0131 (5) | 0.0250 (6) | 0.0258 (6) | 0.000 | −0.0039 (4) | 0.000 |
O1 | 0.044 (2) | 0.034 (2) | 0.066 (3) | 0.002 (2) | −0.024 (2) | 0.007 (2) |
O2 | 0.024 (3) | 0.047 (4) | 0.042 (4) | 0.002 (3) | −0.009 (3) | −0.004 (3) |
O1W | 0.029 (2) | 0.042 (2) | 0.093 (3) | −0.012 (2) | −0.025 (2) | 0.030 (2) |
O2W | 0.032 (3) | 0.133 (6) | 0.029 (3) | 0.000 | −0.007 (2) | 0.000 |
N1 | 0.028 (4) | 0.032 (4) | 0.043 (5) | 0.002 (3) | −0.016 (3) | 0.000 (4) |
C1 | 0.025 (5) | 0.032 (5) | 0.033 (5) | 0.003 (4) | −0.010 (4) | 0.001 (4) |
C2 | 0.023 (3) | 0.041 (6) | 0.025 (3) | 0.013 (7) | −0.004 (2) | 0.002 (6) |
C3 | 0.034 (6) | 0.033 (6) | 0.033 (5) | 0.009 (5) | −0.001 (4) | −0.007 (4) |
C4 | 0.033 (6) | 0.026 (6) | 0.043 (7) | 0.005 (4) | −0.003 (5) | −0.005 (5) |
C5 | 0.027 (5) | 0.034 (5) | 0.029 (5) | 0.009 (3) | −0.005 (4) | 0.003 (3) |
C6 | 0.030 (3) | 0.031 (3) | 0.027 (3) | 0.000 | −0.008 (2) | 0.000 |
Geometric parameters (Å, º) top
Co1—O1W | 2.042 (3) | C3—C4 | 1.385 (9) |
Co1—O1Wi | 2.042 (3) | C4—C5 | 1.408 (8) |
Co1—O1Wii | 2.042 (3) | C6—O1iii | 1.245 (4) |
Co1—O1Wiii | 2.042 (3) | C6—C2iii | 1.510 (9) |
Co1—O2W | 2.113 (5) | O2—H2O | 0.85 |
Co1—O2Wii | 2.113 (5) | O1W—H1W1 | 0.85 (1) |
O1—C6 | 1.245 (4) | O1W—H1W2 | 0.84 (1) |
O2—C5 | 1.28 (1) | O2W—H2W1 | 0.85 (1) |
N1—C1 | 1.358 (9) | O2W—H2W2 | 0.85 (1) |
N1—C5 | 1.366 (8) | C1—H1 | 0.93 |
C1—C2 | 1.383 (9) | C3—H3 | 0.93 |
C2—C3 | 1.381 (9) | C4—H4 | 0.93 |
C2—C6 | 1.510 (9) | | |
| | | |
O1Wii—Co1—O1W | 180.0 | C3—C4—C5 | 119.3 (9) |
O1Wii—Co1—O1Wi | 88.1 (2) | O2—C5—N1 | 118.6 (8) |
O1W—Co1—O1Wi | 91.9 (2) | O2—C5—C4 | 124.1 (7) |
O1Wii—Co1—O1Wiii | 91.9 (2) | N1—C5—C4 | 117.3 (8) |
O1W—Co1—O1Wiii | 88.1 (2) | O1iii—C6—O1 | 125.2 (6) |
O1Wi—Co1—O1Wiii | 180 | O1iii—C6—C2 | 122.1 (6) |
O1Wii—Co1—O2Wii | 91.9 (2) | O1—C6—C2 | 112.6 (6) |
O1W—Co1—O2Wii | 88.2 (2) | O1iii—C6—C2iii | 112.6 (6) |
O1Wi—Co1—O2Wii | 91.9 (2) | O1—C6—C2iii | 122.1 (6) |
O1Wiii—Co1—O2Wii | 88.2 (2) | Co1—O1W—H1W1 | 116 (3) |
O1Wii—Co1—O2W | 88.2 (2) | Co1—O1W—H1W2 | 133 (3) |
O1W—Co1—O2W | 91.9 (2) | H1W1—O1W—H1W2 | 111 (2) |
O1Wi—Co1—O2W | 88.2 (2) | Co1—O2W—H2W1 | 123 (5) |
O1Wiii—Co1—O2W | 91.9 (2) | Co1—O2W—H2W2 | 127 (5) |
O2Wii—Co1—O2W | 180 | H2W1—O2W—H2W2 | 110 (2) |
C1—N1—C5 | 123.2 (9) | N1—C1—H1 | 119.8 |
N1—C1—C2 | 120.4 (8) | C2—C1—H1 | 119.8 |
C3—C2—C1 | 117.7 (8) | C2—C3—H3 | 119.0 |
C3—C2—C6 | 123.9 (9) | C4—C3—H3 | 119.0 |
C1—C2—C6 | 118.4 (9) | C3—C4—H4 | 120.3 |
C2—C3—C4 | 122.0 (9) | C5—C4—H4 | 120.3 |
| | | |
C5—N1—C1—C2 | 0.1 (3) | C3—C4—C5—O2 | −179.9 (8) |
N1—C1—C2—C3 | 0.1 (3) | C3—C4—C5—N1 | 0.4 (8) |
N1—C1—C2—C6 | 178.6 (6) | C3—C2—C6—O1iii | 10.6 (9) |
C1—C2—C3—C4 | 0.0 (6) | C1—C2—C6—O1iii | −167.8 (5) |
C6—C2—C3—C4 | −178.5 (7) | C3—C2—C6—O1 | −169.5 (6) |
C2—C3—C4—C5 | −0.2 (8) | C1—C2—C6—O1 | 12.0 (7) |
C1—N1—C5—O2 | 179.9 (7) | C3—C2—C6—C2iii | 10.6 (5) |
C1—N1—C5—C4 | −0.4 (6) | C1—C2—C6—C2iii | −167.9 (4) |
Symmetry codes: (i) −x+1, y, −z+1; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O1 | 0.85 (1) | 1.83 (2) | 2.659 (4) | 168 (4) |
O1W—H1W2···O1iv | 0.84 (1) | 1.87 (1) | 2.710 (5) | 171 (5) |
O2W—H2W1···O2v | 0.85 (1) | 2.02 (3) | 2.791 (8) | 151 (4) |
O2W—H2W1···O2v | 0.85 (1) | 2.02 (3) | 2.791 (8) | 151 (4) |
O2W—H2W2···O2vi | 0.85 (1) | 1.97 (1) | 2.769 (9) | 157 (2) |
O2W—H2W2···O2vii | 0.85 (1) | 1.97 (1) | 2.769 (9) | 157 (2) |
O2—H2O···N1viii | 0.85 | 2.04 | 2.86 (1) | 159 |
Symmetry codes: (iv) −x+3/2, −y+3/2, −z+1; (v) x−1, y, z−1; (vi) −x+2, −y+1, −z+1; (vii) −x+2, y, −z+1; (viii) −x+5/2, −y+3/2, −z+2. |
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