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The crystal structure of the title compound, [Co(H2O)6](C8H5O3)2·2H2O, consists of octa­hedral CoII complex cations that inter­act with the anions and uncoordinated water mol­ecules, forming a tightly held, hydrogen-bonded layer. The CoII complex cation lies on a special position of site symmetry \overline{1}.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806048094/xu2165sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806048094/xu2165Isup2.hkl
Contains datablock I

CCDC reference: 630531

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](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

Computing details top

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).

(I) top
Crystal data top
[Co(H2O)6](C8H5O3)2·2H2OZ = 1
Mr = 501.30F(000) = 261
Triclinic, P1Dx = 1.547 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.3470 (3) ÅCell parameters from 7354 reflections
b = 7.4194 (4) Åθ = 3.0–27.5°
c = 12.5041 (7) ŵ = 0.87 mm1
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 tube2325 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.017
ω scansθmax = 27.5°, θmin = 3.0°
Absorption correction: multi-scan
ABSCOR (Higashi, 1995)
h = 88
Tmin = 0.614, Tmax = 0.860k = 89
5333 measured reflectionsl = 1616
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)] = 0.029Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.080H 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 parametersΔρmax = 0.55 e Å3
26 restraintsΔρmin = 0.27 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Co10.50000.50000.50000.02477 (10)
O11.0801 (2)0.7127 (2)0.31624 (10)0.0444 (3)
O21.4155 (3)0.7812 (3)0.23950 (13)0.0690 (5)
O30.6234 (3)0.7341 (3)0.19571 (13)0.0695 (5)
O1w0.66853 (19)0.71849 (18)0.38795 (9)0.0324 (2)
O2w0.1868 (2)0.44728 (19)0.42657 (11)0.0376 (3)
O3w0.5189 (3)0.2767 (2)0.40160 (11)0.0461 (3)
O4w0.8068 (2)1.11416 (18)0.47578 (11)0.0399 (3)
C11.2085 (3)0.7485 (3)0.23584 (14)0.0361 (4)
C21.1044 (3)0.7512 (2)0.12764 (13)0.0303 (3)
C30.8695 (8)0.6630 (5)0.1103 (4)0.0354 (8)0.52 (1)
C40.7815 (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
C50.9189 (3)0.7571 (2)0.07296 (13)0.0373 (4)
C61.1603 (8)0.8490 (6)0.0546 (4)0.0417 (9)0.52 (1)
C71.2536 (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
C80.8198 (4)0.7654 (3)0.17807 (16)0.0515 (5)
H30.77190.60080.16530.043*0.52 (1)
H40.62280.60920.00090.046*0.52 (1)
H3'0.79230.73570.17790.043*0.48
H4'0.63620.73650.01010.046*0.48
H61.25680.91120.11000.050*0.52 (1)
H71.41180.90720.05840.043*0.52 (1)
H6'1.21760.76520.12680.050*0.48
H7'1.37280.76200.03940.043*0.48
H80.91900.79780.23570.062*
H1w10.781 (3)0.710 (3)0.3562 (16)0.040 (6)*
H1w20.585 (4)0.735 (4)0.3402 (16)0.063 (7)*
H2w10.146 (4)0.531 (3)0.3986 (18)0.051 (6)*
H2w20.073 (3)0.341 (2)0.4358 (19)0.051 (6)*
H3w10.480 (4)0.256 (4)0.3364 (9)0.063 (7)*
H3w20.603 (3)0.219 (3)0.4167 (19)0.052 (7)*
H4w10.816 (4)1.130 (4)0.5428 (8)0.060 (7)*
H4w20.772 (4)0.9953 (17)0.4591 (18)0.047 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.02564 (16)0.02809 (16)0.02346 (15)0.01360 (11)0.00254 (10)0.00390 (10)
O10.0385 (7)0.0688 (9)0.0326 (6)0.0272 (6)0.0024 (5)0.0170 (6)
O20.0388 (7)0.1292 (16)0.0518 (9)0.0436 (9)0.0041 (6)0.0418 (10)
O30.0748 (11)0.0966 (13)0.0396 (8)0.0383 (10)0.0246 (8)0.0068 (8)
O1w0.0283 (6)0.0419 (6)0.0299 (6)0.0162 (5)0.0001 (4)0.0110 (5)
O2w0.0281 (6)0.0388 (6)0.0462 (7)0.0126 (5)0.0054 (5)0.0144 (5)
O3w0.0690 (9)0.0577 (8)0.0310 (6)0.0466 (7)0.0140 (6)0.0087 (6)
O4w0.0404 (7)0.0317 (6)0.0464 (8)0.0131 (5)0.0057 (6)0.0054 (5)
C10.0346 (8)0.0451 (9)0.0350 (8)0.0215 (7)0.0005 (7)0.0147 (7)
C20.0333 (8)0.0317 (7)0.0302 (8)0.0171 (6)0.0007 (6)0.0066 (6)
C30.0327 (10)0.038 (2)0.0326 (11)0.0101 (19)0.0001 (8)0.007 (2)
C40.0348 (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)
C50.0508 (10)0.0363 (8)0.0293 (8)0.0225 (7)0.0066 (7)0.0023 (6)
C60.0502 (16)0.052 (3)0.0298 (13)0.028 (2)0.0074 (11)0.006 (2)
C70.0304 (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)
C80.0707 (14)0.0588 (12)0.0313 (9)0.0332 (11)0.0081 (9)0.0040 (8)
Geometric parameters (Å, º) top
Co1—O1w2.127 (1)C3—C41.377 (6)
Co1—O2w2.071 (1)C3—H30.9300
Co1—O3w2.065 (1)C4—C51.370 (5)
O1—C11.262 (2)C4—H40.9300
O2—C11.236 (2)C3'—C4'1.387 (6)
O3—C81.191 (3)C3'—H3'0.9300
O1w—H1w10.84 (1)C4'—C51.391 (5)
O1w—H1w20.85 (1)C4'—H4'0.9300
O2w—H2w10.85 (1)C5—C6'1.351 (5)
O2w—H2w20.84 (1)C5—C61.417 (5)
O3w—H3w10.84 (1)C5—C81.471 (2)
O3w—H3w20.84 (1)C6—C71.392 (5)
O4w—H4w10.84 (1)C6—H60.9300
O4w—H4w20.84 (1)C7—H70.9300
C1—C21.510 (2)C6'—C7'1.384 (6)
C2—C31.378 (5)C6'—H6'0.9300
C2—C7'1.385 (5)C7'—H7'0.9300
C2—C71.402 (4)C8—H80.9300
C2—C3'1.411 (5)
O1w—Co1—O1wi180C5—C4—C3122.4 (4)
O1w—Co1—O2w89.57 (5)C5—C4—H4118.8
O1w—Co1—O2wi90.43 (5)C3—C4—H4118.8
O1w—Co1—O3w92.73 (6)C4'—C3'—C2120.7 (5)
O1w—Co1—O3wi87.27 (6)C4'—C3'—H3'119.6
O2w—Co1—O2wi180C2—C3'—H3'119.6
O2w—Co1—O3w88.04 (6)C5—C4'—C3'118.8 (5)
O2w—Co1—O3wi91.96 (5)C5—C4'—H4'120.6
O3w—Co1—O3wi180C3'—C4'—H4'120.6
Co1—O1w—H1w1116.7 (15)C6'—C5—C4113.4 (3)
Co1—O1w—H1w2116.8 (18)C6'—C5—C4'121.7 (3)
H1w1—O1w—H1w2106 (2)C4—C5—C6118.4 (3)
Co1—O2w—H2w1127.5 (17)C4'—C5—C6115.4 (3)
Co1—O2w—H2w2119.7 (17)C6'—C5—C8120.2 (3)
H2w1—O2w—H2w2111 (2)C4—C5—C8121.3 (3)
Co1—O3w—H3w1125.6 (18)C4'—C5—C8118.1 (3)
Co1—O3w—H3w2122.0 (17)C6—C5—C8120.3 (3)
H3w1—O3w—H3w2110 (2)C7—C6—C5120.3 (4)
H4w1—O4w—H4w2109 (2)C7—C6—H6119.9
O2—C1—O1124.26 (17)C5—C6—H6119.9
O2—C1—C2117.34 (15)C6—C7—C2118.7 (4)
O1—C1—C2118.40 (14)C6—C7—H7120.6
C3—C2—C7'112.2 (3)C2—C7—H7120.6
C3—C2—C7121.2 (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—C1120.8 (2)C6'—C7'—C2122.2 (4)
C7'—C2—C1121.2 (2)C6'—C7'—H7'118.9
C7—C2—C1118.0 (2)C2—C7'—H7'118.9
C3'—C2—C1121.5 (3)O3—C8—C5125.6 (2)
C2—C3—C4119.0 (4)O3—C8—H8117.2
C2—C3—H3120.5C5—C8—H8117.2
C4—C3—H3120.5
O2—C1—C2—C3161.1 (2)C3'—C4'—C5—C625.7 (3)
O1—C1—C2—C318.6 (3)C3'—C4'—C5—C8177.95 (17)
O2—C1—C2—C7'10.0 (3)C6'—C5—C6—C784.6 (9)
O1—C1—C2—C7'169.7 (2)C4—C5—C6—C70.5 (4)
O2—C1—C2—C719.1 (3)C4'—C5—C6—C726.4 (4)
O1—C1—C2—C7161.1 (2)C8—C5—C6—C7177.9 (3)
O2—C1—C2—C3'171.2 (2)C5—C6—C7—C20.3 (5)
O1—C1—C2—C3'9.0 (3)C3—C2—C7—C60.8 (4)
C7'—C2—C3—C426.3 (2)C7'—C2—C7—C675.2 (8)
C7—C2—C3—C40.5 (2)C3'—C2—C7—C626.6 (4)
C3'—C2—C3—C481.3 (9)C1—C2—C7—C6179.5 (3)
C1—C2—C3—C4179.81 (17)C4—C5—C6'—C7'26.7 (4)
C2—C3—C4—C50.4 (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'—C20.4 (5)
C1—C2—C3'—C4'179.65 (17)C3—C2—C7'—C6'26.5 (4)
C2—C3'—C4'—C50.9 (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—C60.9 (3)C6'—C5—C8—O3168.3 (3)
C3—C4—C5—C8178.26 (17)C4—C5—C8—O315.2 (3)
C3'—C4'—C5—C6'2.5 (4)C4'—C5—C8—O311.3 (3)
C3'—C4'—C5—C477.6 (10)C6—C5—C8—O3162.1 (3)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O10.84 (1)1.95 (1)2.778 (2)166 (2)
O1w—H1w2···O2ii0.85 (1)1.78 (1)2.629 (2)178 (3)
O2w—H2w1···O1ii0.85 (1)1.90 (1)2.746 (2)171 (2)
O2w—H2w2···O4wiii0.84 (1)1.93 (1)2.760 (2)172 (2)
O3w—H3w1···O3iv0.84 (1)1.89 (1)2.715 (2)165 (3)
O3w—H3w2···O4wv0.84 (1)1.92 (1)2.743 (2)169 (2)
O4w—H4w1···O1vi0.84 (1)2.03 (2)2.812 (2)155 (3)
O4w—H4w2···O1w0.84 (1)2.05 (1)2.872 (2)168 (2)
Symmetry codes: (ii) x1, y, z; (iii) x1, y1, z; (iv) x+1, y+1, z; (v) x, y1, z; (vi) x+2, y+2, z+1.
 

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