The Co
III atom in the title compound, [Co(C
2H
8N
2)
2(OH)(H
2O)](C
10H
6O
6S
2)·H
2O, exhibits an octahedral coordination geometry, with the hydroxide and water ligands occupying
cis sites. Adjacent cations are linked into linear chains through hydrogen-bonded OH
OH
2 units. The Co
III atom lies on a twofold rotation axis and the naphthalene-1,5-disulfonate dianion lies on a centre of inversion.
Supporting information
CCDC reference: 640254
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- Disorder in main residue
- R factor = 0.040
- wR factor = 0.105
- Data-to-parameter ratio = 15.5
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT395_ALERT_2_B Deviating X-O-Y Angle from 120 Deg for <O1W' 162.00 Deg.
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98
PLAT301_ALERT_3_C Main Residue Disorder ......................... 4.00 Perc.
PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O1W
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 1
O1 -CO1 -N1 -C1 9.10 1.70 1.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 8
N2 -CO1 -N2 -C2 115.71 0.19 2.655 1.555 1.555 1.555
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 5
Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
7 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
3 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
1 ALERT type 3 Indicator that the structure quality may be low
4 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
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: X-SEED (Barbour, 2001); software used to prepare material for publication: SHELXL97 and publCIF (Westrip, 2007).
Aquabis(1,2-ethanediamine-
κ2N,
N')hydroxidocobalt(III)
naphthalene-1,5-disulfonate monohydrate
top
Crystal data top
[Co(C2H8N2)2(OH)(H2O)](C10H6O6S2)·H2O | F(000) = 1080 |
Mr = 518.45 | Dx = 1.607 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 2369 reflections |
a = 21.017 (2) Å | θ = 3.0–26.9° |
b = 11.0917 (8) Å | µ = 1.05 mm−1 |
c = 9.2140 (7) Å | T = 293 K |
β = 94.002 (1)° | Block, orange |
V = 2142.7 (3) Å3 | 0.41 × 0.33 × 0.28 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 2336 independent reflections |
Radiation source: fine-focus sealed tube | 1714 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.047 |
φ and ω scans | θmax = 27.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −26→26 |
Tmin = 0.673, Tmax = 0.758 | k = −14→14 |
8917 measured reflections | l = −11→11 |
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)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.105 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0493P)2 + 2.9275P] where P = (Fo2 + 2Fc2)/3 |
2336 reflections | (Δ/σ)max = 0.001 |
151 parameters | Δρmax = 0.46 e Å−3 |
15 restraints | Δρmin = −0.36 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 | 0.37103 (5) | 0.2500 | 0.02094 (17) | |
S1 | 0.38767 (4) | 0.25322 (7) | −0.27412 (9) | 0.0290 (2) | |
O1 | 0.52879 (10) | 0.48891 (18) | 0.3903 (2) | 0.0267 (5) | |
H1 | 0.4996 | 0.5004 | 0.4476 | 0.040* | 0.75 |
H11 | 0.5374 | 0.5553 | 0.3500 | 0.040* | 0.75 |
O2 | 0.40458 (11) | 0.3452 (2) | −0.1658 (3) | 0.0413 (6) | |
O3 | 0.42854 (10) | 0.2566 (2) | −0.3945 (3) | 0.0398 (6) | |
O4 | 0.38309 (11) | 0.1339 (2) | −0.2130 (3) | 0.0389 (6) | |
O1w | 0.5003 (11) | 0.0029 (6) | 0.2811 (13) | 0.046 (5) | 0.297 (7) |
O1w' | 0.4866 (8) | 0.0018 (13) | 0.4204 (19) | 0.072 (6) | 0.203 (7) |
H1w | 0.4768 | −0.0176 | 0.3370 | 0.109* | |
N1 | 0.46598 (12) | 0.2485 (2) | 0.1142 (3) | 0.0273 (6) | |
H1n1 | 0.4635 | 0.2767 | 0.0283 | 0.033* | |
H1n2 | 0.4908 | 0.1879 | 0.1167 | 0.033* | |
N2 | 0.41488 (11) | 0.3747 (2) | 0.3204 (3) | 0.0265 (6) | |
H2n1 | 0.4144 | 0.3351 | 0.3993 | 0.032* | |
H2n2 | 0.4042 | 0.4471 | 0.3370 | 0.032* | |
C1 | 0.40192 (15) | 0.2108 (3) | 0.1540 (4) | 0.0337 (8) | |
H1A | 0.4055 | 0.1494 | 0.2290 | 0.040* | |
H1B | 0.3775 | 0.1782 | 0.0698 | 0.040* | |
C2 | 0.36968 (15) | 0.3209 (3) | 0.2088 (3) | 0.0318 (7) | |
H2A | 0.3601 | 0.3775 | 0.1300 | 0.038* | |
H2B | 0.3302 | 0.2991 | 0.2507 | 0.038* | |
C3 | 0.30995 (14) | 0.2943 (3) | −0.3500 (3) | 0.0279 (7) | |
C4 | 0.28212 (15) | 0.3937 (3) | −0.2970 (4) | 0.0361 (8) | |
H4 | 0.3020 | 0.4340 | −0.2177 | 0.043* | |
C5 | 0.22401 (16) | 0.4365 (3) | −0.3598 (4) | 0.0404 (9) | |
H5 | 0.2057 | 0.5052 | −0.3226 | 0.048* | |
C6 | 0.19402 (15) | 0.3779 (3) | −0.4753 (4) | 0.0332 (7) | |
H6 | 0.1558 | 0.4081 | −0.5176 | 0.040* | |
C7 | 0.22017 (14) | 0.2721 (3) | −0.5312 (3) | 0.0252 (6) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0228 (3) | 0.0232 (3) | 0.0168 (3) | 0.000 | 0.0010 (2) | 0.000 |
S1 | 0.0253 (4) | 0.0324 (5) | 0.0283 (4) | −0.0062 (3) | −0.0051 (3) | 0.0074 (3) |
O1 | 0.0326 (12) | 0.0272 (11) | 0.0210 (11) | −0.0017 (9) | 0.0073 (9) | −0.0045 (9) |
O2 | 0.0425 (14) | 0.0395 (14) | 0.0390 (14) | −0.0075 (11) | −0.0183 (11) | 0.0012 (11) |
O3 | 0.0262 (12) | 0.0555 (16) | 0.0376 (13) | −0.0017 (11) | 0.0013 (10) | 0.0146 (11) |
O4 | 0.0380 (13) | 0.0352 (13) | 0.0424 (14) | −0.0065 (11) | −0.0059 (11) | 0.0149 (11) |
O1W | 0.042 (4) | 0.028 (4) | 0.066 (11) | −0.004 (5) | −0.003 (8) | −0.005 (4) |
O1W' | 0.078 (8) | 0.049 (7) | 0.087 (10) | −0.036 (6) | −0.023 (7) | 0.006 (7) |
N1 | 0.0329 (14) | 0.0282 (14) | 0.0204 (13) | 0.0008 (11) | −0.0007 (11) | −0.0031 (11) |
N2 | 0.0273 (13) | 0.0304 (14) | 0.0220 (13) | 0.0019 (11) | 0.0028 (10) | 0.0034 (11) |
C1 | 0.0342 (18) | 0.0325 (18) | 0.0335 (18) | −0.0107 (14) | −0.0032 (14) | 0.0002 (14) |
C2 | 0.0266 (16) | 0.0384 (19) | 0.0300 (17) | −0.0039 (14) | −0.0006 (13) | 0.0019 (14) |
C3 | 0.0214 (15) | 0.0332 (17) | 0.0286 (16) | −0.0031 (13) | −0.0001 (12) | 0.0013 (13) |
C4 | 0.0315 (17) | 0.039 (2) | 0.0370 (19) | −0.0044 (15) | −0.0031 (14) | −0.0126 (15) |
C5 | 0.0352 (19) | 0.0330 (19) | 0.053 (2) | 0.0065 (15) | 0.0004 (16) | −0.0139 (17) |
C6 | 0.0237 (16) | 0.0360 (19) | 0.0395 (19) | 0.0032 (14) | −0.0012 (13) | −0.0027 (15) |
C7 | 0.0221 (15) | 0.0262 (16) | 0.0273 (16) | −0.0022 (12) | 0.0027 (12) | −0.0001 (12) |
Geometric parameters (Å, º) top
Co1—O1 | 1.908 (2) | N2—H2N1 | 0.850 |
Co1—O1i | 1.908 (2) | N2—H2N2 | 0.850 |
Co1—N1 | 1.949 (2) | C1—C2 | 1.501 (4) |
Co1—N1i | 1.949 (2) | C1—H1A | 0.970 |
Co1—N2 | 1.946 (2) | C1—H1B | 0.970 |
Co1—N2i | 1.946 (2) | C2—H2A | 0.970 |
S1—O4 | 1.444 (2) | C2—H2B | 0.970 |
S1—O3 | 1.450 (2) | C3—C4 | 1.355 (4) |
S1—O2 | 1.454 (2) | C3—C7ii | 1.430 (4) |
S1—C3 | 1.790 (3) | C4—C5 | 1.397 (5) |
O1—H1 | 0.85 | C4—H4 | 0.930 |
O1—H11 | 0.85 | C5—C6 | 1.363 (4) |
O1W—H1W | 0.77 | C5—H5 | 0.930 |
O1W'—H1W | 0.81 | C6—C7 | 1.408 (4) |
N1—C1 | 1.480 (4) | C6—H6 | 0.930 |
N1—H1N1 | 0.850 | C7—C7ii | 1.429 (6) |
N1—H1N2 | 0.850 | C7—C3ii | 1.430 (4) |
N2—C2 | 1.477 (4) | | |
| | | |
O1—Co1—O1i | 93.5 (1) | H2N1—N2—H2N2 | 108.3 |
O1—Co1—N1 | 176.3 (1) | N1—C1—C2 | 107.0 (2) |
O1i—Co1—N1 | 87.6 (1) | N1—C1—H1A | 110.3 |
O1—Co1—N2 | 90.9 (1) | C2—C1—H1A | 110.3 |
O1i—Co1—N2 | 87.5 (1) | N1—C1—H1B | 110.3 |
N1—Co1—N1i | 91.6 (2) | C2—C1—H1B | 110.3 |
N1—Co1—N2 | 85.6 (1) | H1A—C1—H1B | 108.6 |
N1—Co1—N2i | 96.0 (1) | N2—C2—C1 | 106.2 (2) |
N2—Co1—N2i | 177.6 (2) | N2—C2—H2A | 110.5 |
O4—S1—O3 | 112.41 (15) | C1—C2—H2A | 110.5 |
O4—S1—O2 | 113.26 (14) | N2—C2—H2B | 110.5 |
O3—S1—O2 | 112.19 (15) | C1—C2—H2B | 110.5 |
O4—S1—C3 | 107.56 (14) | H2A—C2—H2B | 108.7 |
O3—S1—C3 | 105.53 (14) | C4—C3—C7ii | 121.1 (3) |
O2—S1—C3 | 105.20 (14) | C4—C3—S1 | 118.1 (2) |
Co1—O1—H1 | 108.40 (16) | C7ii—C3—S1 | 120.7 (2) |
Co1—O1—H11 | 111.37 (16) | C3—C4—C5 | 120.9 (3) |
H1—O1—H11 | 109.1 (2) | C3—C4—H4 | 119.6 |
C1—N1—Co1 | 109.73 (19) | C5—C4—H4 | 119.6 |
C1—N1—H1N1 | 109.7 | C6—C5—C4 | 120.3 (3) |
Co1—N1—H1N1 | 109.7 | C6—C5—H5 | 119.8 |
C1—N1—H1N2 | 109.7 | C4—C5—H5 | 119.8 |
Co1—N1—H1N2 | 109.7 | C5—C6—C7 | 120.8 (3) |
H1N1—N1—H1N2 | 108.2 | C5—C6—H6 | 119.6 |
C2—N2—Co1 | 108.71 (18) | C7—C6—H6 | 119.6 |
C2—N2—H2N1 | 109.9 | C6—C7—C7ii | 119.5 (3) |
Co1—N2—H2N1 | 109.9 | C6—C7—C3ii | 123.1 (3) |
C2—N2—H2N2 | 109.9 | C7ii—C7—C3ii | 117.4 (3) |
Co1—N2—H2N2 | 109.9 | | |
| | | |
O1—Co1—N1—C1 | 9.1 (17) | O4—S1—C3—C4 | 120.0 (3) |
O1i—Co1—N1—C1 | −97.6 (2) | O3—S1—C3—C4 | −119.8 (3) |
N2—Co1—N1—C1 | −9.9 (2) | O2—S1—C3—C4 | −1.0 (3) |
N2i—Co1—N1—C1 | 171.8 (2) | O4—S1—C3—C7ii | −63.5 (3) |
N1i—Co1—N1—C1 | 86.0 (2) | O3—S1—C3—C7ii | 56.7 (3) |
O1—Co1—N2—C2 | 162.40 (19) | O2—S1—C3—C7ii | 175.5 (2) |
O1i—Co1—N2—C2 | 68.97 (19) | C7ii—C3—C4—C5 | −2.0 (5) |
N2i—Co1—N2—C2 | 115.71 (19) | S1—C3—C4—C5 | 174.5 (3) |
N1—Co1—N2—C2 | −18.8 (2) | C3—C4—C5—C6 | 0.6 (6) |
N1i—Co1—N2—C2 | −109.9 (2) | C4—C5—C6—C7 | 1.4 (5) |
Co1—N1—C1—C2 | 36.0 (3) | C5—C6—C7—C7ii | −1.9 (6) |
Co1—N2—C2—C1 | 42.9 (3) | C5—C6—C7—C3ii | 178.6 (3) |
N1—C1—C2—N2 | −51.1 (3) | | |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) −x+1/2, −y+1/2, −z−1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O1iii | 0.85 | 1.65 | 2.439 (4) | 154 |
O1—H11···O3iv | 0.85 | 2.24 | 2.961 (3) | 144 |
N1—H1N1···O2 | 0.85 | 2.24 | 3.001 (3) | 150 |
N1—H1N2···O1Wi | 0.85 | 2.26 | 2.960 (9) | 140 |
N1—H1N2···O1W'i | 0.85 | 2.15 | 2.94 (1) | 154 |
N2—H2N1···O3v | 0.85 | 2.09 | 2.932 (3) | 169 |
N2—H2N2···O2vi | 0.85 | 2.30 | 3.118 (4) | 160 |
Symmetry codes: (i) −x+1, y, −z+1/2; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y+1, −z; (v) x, y, z+1; (vi) x, −y+1, z+1/2. |