The crystal structure of the title compound, [Co(H
2O)
6](C
8H
5O
3)
2·2H
2O, consists of octahedral Co
II complex cations that interact with the anions and uncoordinated water molecules, forming a tightly held, hydrogen-bonded layer. The Co
II complex cation lies on a special position of site symmetry
.
Supporting information
CCDC reference: 630531
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.003 Å
- Disorder in main residue
- R factor = 0.029
- wR factor = 0.080
- Data-to-parameter ratio = 13.1
checkCIF/PLATON results
No syntax errors found
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.614 0.860
Tmin(prime) and Tmax expected: 0.727 0.856
RR(prime) = 0.840
Please check that your absorption correction is appropriate.
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.83
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.04
PLAT301_ALERT_3_C Main Residue Disorder ......................... 17.00 Perc.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 8
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3
H2 O
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
6 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
2 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: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2006).
Crystal data top
[Co(H2O)6](C8H5O3)2·2H2O | Z = 1 |
Mr = 501.30 | F(000) = 261 |
Triclinic, P1 | Dx = 1.547 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.3470 (3) Å | Cell parameters from 7354 reflections |
b = 7.4194 (4) Å | θ = 3.0–27.5° |
c = 12.5041 (7) Å | µ = 0.87 mm−1 |
α = 92.353 (2)° | T = 295 K |
β = 90.029 (3)° | Prism, pink |
γ = 113.801 (6)° | 0.36 × 0.28 × 0.18 mm |
V = 538.20 (5) Å3 | |
Data collection top
Rigaku RAXIS-RAPID IP diffractometer | 2451 independent reflections |
Radiation source: fine-focus sealed tube | 2325 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.017 |
ω scans | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan ABSCOR (Higashi, 1995) | h = −8→8 |
Tmin = 0.614, Tmax = 0.860 | k = −8→9 |
5333 measured reflections | l = −16→16 |
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)] = 0.029 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.080 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0485P)2 + 0.2223P] where P = (Fo2 + 2Fc2)/3 |
2451 reflections | (Δ/σ)max = 0.001 |
187 parameters | Δρmax = 0.55 e Å−3 |
26 restraints | Δρmin = −0.27 e Å−3 |
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 | 0.02477 (10) | |
O1 | 1.0801 (2) | 0.7127 (2) | 0.31624 (10) | 0.0444 (3) | |
O2 | 1.4155 (3) | 0.7812 (3) | 0.23950 (13) | 0.0690 (5) | |
O3 | 0.6234 (3) | 0.7341 (3) | −0.19571 (13) | 0.0695 (5) | |
O1w | 0.66853 (19) | 0.71849 (18) | 0.38795 (9) | 0.0324 (2) | |
O2w | 0.1868 (2) | 0.44728 (19) | 0.42657 (11) | 0.0376 (3) | |
O3w | 0.5189 (3) | 0.2767 (2) | 0.40160 (11) | 0.0461 (3) | |
O4w | 0.8068 (2) | 1.11416 (18) | 0.47578 (11) | 0.0399 (3) | |
C1 | 1.2085 (3) | 0.7485 (3) | 0.23584 (14) | 0.0361 (4) | |
C2 | 1.1044 (3) | 0.7512 (2) | 0.12764 (13) | 0.0303 (3) | |
C3 | 0.8695 (8) | 0.6630 (5) | 0.1103 (4) | 0.0354 (8) | 0.52 (1) |
C4 | 0.7815 (9) | 0.6682 (6) | 0.0104 (4) | 0.0387 (9) | 0.52 (1) |
C3' | 0.8791 (8) | 0.7425 (5) | 0.1171 (4) | 0.0354 (8) | 0.48 |
C4' | 0.7855 (10) | 0.7441 (5) | 0.0170 (4) | 0.0387 (9) | 0.48 |
C5 | 0.9189 (3) | 0.7571 (2) | −0.07296 (13) | 0.0373 (4) | |
C6 | 1.1603 (8) | 0.8490 (6) | −0.0546 (4) | 0.0417 (9) | 0.52 (1) |
C7 | 1.2536 (7) | 0.8467 (6) | 0.0458 (3) | 0.0358 (8) | 0.52 (1) |
C6' | 1.1331 (9) | 0.7610 (6) | −0.0655 (4) | 0.0417 (9) | 0.48 |
C7' | 1.2250 (8) | 0.7586 (6) | 0.0345 (4) | 0.0358 (8) | 0.48 |
C8 | 0.8198 (4) | 0.7654 (3) | −0.17807 (16) | 0.0515 (5) | |
H3 | 0.7719 | 0.6008 | 0.1653 | 0.043* | 0.52 (1) |
H4 | 0.6228 | 0.6092 | −0.0009 | 0.046* | 0.52 (1) |
H3' | 0.7923 | 0.7357 | 0.1779 | 0.043* | 0.48 |
H4' | 0.6362 | 0.7365 | 0.0101 | 0.046* | 0.48 |
H6 | 1.2568 | 0.9112 | −0.1100 | 0.050* | 0.52 (1) |
H7 | 1.4118 | 0.9072 | 0.0584 | 0.043* | 0.52 (1) |
H6' | 1.2176 | 0.7652 | −0.1268 | 0.050* | 0.48 |
H7' | 1.3728 | 0.7620 | 0.0394 | 0.043* | 0.48 |
H8 | 0.9190 | 0.7978 | −0.2357 | 0.062* | |
H1w1 | 0.781 (3) | 0.710 (3) | 0.3562 (16) | 0.040 (6)* | |
H1w2 | 0.585 (4) | 0.735 (4) | 0.3402 (16) | 0.063 (7)* | |
H2w1 | 0.146 (4) | 0.531 (3) | 0.3986 (18) | 0.051 (6)* | |
H2w2 | 0.073 (3) | 0.341 (2) | 0.4358 (19) | 0.051 (6)* | |
H3w1 | 0.480 (4) | 0.256 (4) | 0.3364 (9) | 0.063 (7)* | |
H3w2 | 0.603 (3) | 0.219 (3) | 0.4167 (19) | 0.052 (7)* | |
H4w1 | 0.816 (4) | 1.130 (4) | 0.5428 (8) | 0.060 (7)* | |
H4w2 | 0.772 (4) | 0.9953 (17) | 0.4591 (18) | 0.047 (6)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.02564 (16) | 0.02809 (16) | 0.02346 (15) | 0.01360 (11) | −0.00254 (10) | 0.00390 (10) |
O1 | 0.0385 (7) | 0.0688 (9) | 0.0326 (6) | 0.0272 (6) | 0.0024 (5) | 0.0170 (6) |
O2 | 0.0388 (7) | 0.1292 (16) | 0.0518 (9) | 0.0436 (9) | 0.0041 (6) | 0.0418 (10) |
O3 | 0.0748 (11) | 0.0966 (13) | 0.0396 (8) | 0.0383 (10) | −0.0246 (8) | −0.0068 (8) |
O1w | 0.0283 (6) | 0.0419 (6) | 0.0299 (6) | 0.0162 (5) | −0.0001 (4) | 0.0110 (5) |
O2w | 0.0281 (6) | 0.0388 (6) | 0.0462 (7) | 0.0126 (5) | −0.0054 (5) | 0.0144 (5) |
O3w | 0.0690 (9) | 0.0577 (8) | 0.0310 (6) | 0.0466 (7) | −0.0140 (6) | −0.0087 (6) |
O4w | 0.0404 (7) | 0.0317 (6) | 0.0464 (8) | 0.0131 (5) | −0.0057 (6) | 0.0054 (5) |
C1 | 0.0346 (8) | 0.0451 (9) | 0.0350 (8) | 0.0215 (7) | 0.0005 (7) | 0.0147 (7) |
C2 | 0.0333 (8) | 0.0317 (7) | 0.0302 (8) | 0.0171 (6) | −0.0007 (6) | 0.0066 (6) |
C3 | 0.0327 (10) | 0.038 (2) | 0.0326 (11) | 0.0101 (19) | −0.0001 (8) | 0.007 (2) |
C4 | 0.0348 (10) | 0.040 (3) | 0.0408 (13) | 0.014 (2) | −0.0093 (9) | 0.002 (2) |
C3' | 0.0327 (10) | 0.038 (2) | 0.0326 (11) | 0.0101 (19) | −0.0001 (8) | 0.007 (2) |
C4' | 0.0348 (10) | 0.040 (3) | 0.0408 (13) | 0.014 (2) | −0.0093 (9) | 0.002 (2) |
C5 | 0.0508 (10) | 0.0363 (8) | 0.0293 (8) | 0.0225 (7) | −0.0066 (7) | −0.0023 (6) |
C6 | 0.0502 (16) | 0.052 (3) | 0.0298 (13) | 0.028 (2) | 0.0074 (11) | 0.006 (2) |
C7 | 0.0304 (13) | 0.042 (2) | 0.0381 (14) | 0.0168 (19) | 0.0027 (10) | 0.0076 (19) |
C6' | 0.0502 (16) | 0.052 (3) | 0.0298 (13) | 0.028 (2) | 0.0074 (11) | 0.006 (2) |
C7' | 0.0304 (13) | 0.042 (2) | 0.0381 (14) | 0.0168 (19) | 0.0027 (10) | 0.0076 (19) |
C8 | 0.0707 (14) | 0.0588 (12) | 0.0313 (9) | 0.0332 (11) | −0.0081 (9) | −0.0040 (8) |
Geometric parameters (Å, º) top
Co1—O1w | 2.127 (1) | C3—C4 | 1.377 (6) |
Co1—O2w | 2.071 (1) | C3—H3 | 0.9300 |
Co1—O3w | 2.065 (1) | C4—C5 | 1.370 (5) |
O1—C1 | 1.262 (2) | C4—H4 | 0.9300 |
O2—C1 | 1.236 (2) | C3'—C4' | 1.387 (6) |
O3—C8 | 1.191 (3) | C3'—H3' | 0.9300 |
O1w—H1w1 | 0.84 (1) | C4'—C5 | 1.391 (5) |
O1w—H1w2 | 0.85 (1) | C4'—H4' | 0.9300 |
O2w—H2w1 | 0.85 (1) | C5—C6' | 1.351 (5) |
O2w—H2w2 | 0.84 (1) | C5—C6 | 1.417 (5) |
O3w—H3w1 | 0.84 (1) | C5—C8 | 1.471 (2) |
O3w—H3w2 | 0.84 (1) | C6—C7 | 1.392 (5) |
O4w—H4w1 | 0.84 (1) | C6—H6 | 0.9300 |
O4w—H4w2 | 0.84 (1) | C7—H7 | 0.9300 |
C1—C2 | 1.510 (2) | C6'—C7' | 1.384 (6) |
C2—C3 | 1.378 (5) | C6'—H6' | 0.9300 |
C2—C7' | 1.385 (5) | C7'—H7' | 0.9300 |
C2—C7 | 1.402 (4) | C8—H8 | 0.9300 |
C2—C3' | 1.411 (5) | | |
| | | |
O1w—Co1—O1wi | 180 | C5—C4—C3 | 122.4 (4) |
O1w—Co1—O2w | 89.57 (5) | C5—C4—H4 | 118.8 |
O1w—Co1—O2wi | 90.43 (5) | C3—C4—H4 | 118.8 |
O1w—Co1—O3w | 92.73 (6) | C4'—C3'—C2 | 120.7 (5) |
O1w—Co1—O3wi | 87.27 (6) | C4'—C3'—H3' | 119.6 |
O2w—Co1—O2wi | 180 | C2—C3'—H3' | 119.6 |
O2w—Co1—O3w | 88.04 (6) | C5—C4'—C3' | 118.8 (5) |
O2w—Co1—O3wi | 91.96 (5) | C5—C4'—H4' | 120.6 |
O3w—Co1—O3wi | 180 | C3'—C4'—H4' | 120.6 |
Co1—O1w—H1w1 | 116.7 (15) | C6'—C5—C4 | 113.4 (3) |
Co1—O1w—H1w2 | 116.8 (18) | C6'—C5—C4' | 121.7 (3) |
H1w1—O1w—H1w2 | 106 (2) | C4—C5—C6 | 118.4 (3) |
Co1—O2w—H2w1 | 127.5 (17) | C4'—C5—C6 | 115.4 (3) |
Co1—O2w—H2w2 | 119.7 (17) | C6'—C5—C8 | 120.2 (3) |
H2w1—O2w—H2w2 | 111 (2) | C4—C5—C8 | 121.3 (3) |
Co1—O3w—H3w1 | 125.6 (18) | C4'—C5—C8 | 118.1 (3) |
Co1—O3w—H3w2 | 122.0 (17) | C6—C5—C8 | 120.3 (3) |
H3w1—O3w—H3w2 | 110 (2) | C7—C6—C5 | 120.3 (4) |
H4w1—O4w—H4w2 | 109 (2) | C7—C6—H6 | 119.9 |
O2—C1—O1 | 124.26 (17) | C5—C6—H6 | 119.9 |
O2—C1—C2 | 117.34 (15) | C6—C7—C2 | 118.7 (4) |
O1—C1—C2 | 118.40 (14) | C6—C7—H7 | 120.6 |
C3—C2—C7' | 112.2 (3) | C2—C7—H7 | 120.6 |
C3—C2—C7 | 121.2 (3) | C5—C6'—C7' | 119.1 (4) |
C7'—C2—C3' | 117.3 (3) | C5—C6'—H6' | 120.4 |
C7—C2—C3' | 114.8 (3) | C7'—C6'—H6' | 120.4 |
C3—C2—C1 | 120.8 (2) | C6'—C7'—C2 | 122.2 (4) |
C7'—C2—C1 | 121.2 (2) | C6'—C7'—H7' | 118.9 |
C7—C2—C1 | 118.0 (2) | C2—C7'—H7' | 118.9 |
C3'—C2—C1 | 121.5 (3) | O3—C8—C5 | 125.6 (2) |
C2—C3—C4 | 119.0 (4) | O3—C8—H8 | 117.2 |
C2—C3—H3 | 120.5 | C5—C8—H8 | 117.2 |
C4—C3—H3 | 120.5 | | |
| | | |
O2—C1—C2—C3 | 161.1 (2) | C3'—C4'—C5—C6 | −25.7 (3) |
O1—C1—C2—C3 | −18.6 (3) | C3'—C4'—C5—C8 | −177.95 (17) |
O2—C1—C2—C7' | 10.0 (3) | C6'—C5—C6—C7 | −84.6 (9) |
O1—C1—C2—C7' | −169.7 (2) | C4—C5—C6—C7 | 0.5 (4) |
O2—C1—C2—C7 | −19.1 (3) | C4'—C5—C6—C7 | 26.4 (4) |
O1—C1—C2—C7 | 161.1 (2) | C8—C5—C6—C7 | 177.9 (3) |
O2—C1—C2—C3' | −171.2 (2) | C5—C6—C7—C2 | 0.3 (5) |
O1—C1—C2—C3' | 9.0 (3) | C3—C2—C7—C6 | −0.8 (4) |
C7'—C2—C3—C4 | −26.3 (2) | C7'—C2—C7—C6 | 75.2 (8) |
C7—C2—C3—C4 | 0.5 (2) | C3'—C2—C7—C6 | −26.6 (4) |
C3'—C2—C3—C4 | 81.3 (9) | C1—C2—C7—C6 | 179.5 (3) |
C1—C2—C3—C4 | −179.81 (17) | C4—C5—C6'—C7' | −26.7 (4) |
C2—C3—C4—C5 | 0.4 (2) | C4'—C5—C6'—C7' | −2.2 (5) |
C3—C2—C3'—C4' | −84.0 (9) | C6—C5—C6'—C7' | 80.5 (8) |
C7'—C2—C3'—C4' | −0.83 (19) | C8—C5—C6'—C7' | 178.2 (3) |
C7—C2—C3'—C4' | 27.4 (2) | C5—C6'—C7'—C2 | 0.4 (5) |
C1—C2—C3'—C4' | −179.65 (17) | C3—C2—C7'—C6' | 26.5 (4) |
C2—C3'—C4'—C5 | −0.9 (2) | C7—C2—C7'—C6' | −89.7 (8) |
C3—C4—C5—C6' | 27.0 (3) | C3'—C2—C7'—C6' | 1.1 (4) |
C3—C4—C5—C4' | −89.4 (10) | C1—C2—C7'—C6' | 179.9 (3) |
C3—C4—C5—C6 | −0.9 (3) | C6'—C5—C8—O3 | 168.3 (3) |
C3—C4—C5—C8 | −178.26 (17) | C4—C5—C8—O3 | 15.2 (3) |
C3'—C4'—C5—C6' | 2.5 (4) | C4'—C5—C8—O3 | −11.3 (3) |
C3'—C4'—C5—C4 | 77.6 (10) | C6—C5—C8—O3 | −162.1 (3) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O1 | 0.84 (1) | 1.95 (1) | 2.778 (2) | 166 (2) |
O1w—H1w2···O2ii | 0.85 (1) | 1.78 (1) | 2.629 (2) | 178 (3) |
O2w—H2w1···O1ii | 0.85 (1) | 1.90 (1) | 2.746 (2) | 171 (2) |
O2w—H2w2···O4wiii | 0.84 (1) | 1.93 (1) | 2.760 (2) | 172 (2) |
O3w—H3w1···O3iv | 0.84 (1) | 1.89 (1) | 2.715 (2) | 165 (3) |
O3w—H3w2···O4wv | 0.84 (1) | 1.92 (1) | 2.743 (2) | 169 (2) |
O4w—H4w1···O1vi | 0.84 (1) | 2.03 (2) | 2.812 (2) | 155 (3) |
O4w—H4w2···O1w | 0.84 (1) | 2.05 (1) | 2.872 (2) | 168 (2) |
Symmetry codes: (ii) x−1, y, z; (iii) x−1, y−1, z; (iv) −x+1, −y+1, −z; (v) x, y−1, z; (vi) −x+2, −y+2, −z+1. |