Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807017746/ng2246sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807017746/ng2246Isup2.hkl |
CCDC reference: 646632
Key indicators
- Single-crystal X-ray study
- T = 193 K
- Mean (C-C) = 0.005 Å
- R factor = 0.051
- wR factor = 0.103
- Data-to-parameter ratio = 12.6
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT417_ALERT_2_C Short Inter D-H..H-D H8A .. H11A .. 2.10 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 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 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Cobalt nitrate hydrate (0.2 mmol), 5-benzoyl-4-hydroxy-2-mehtoxybenzenesulfonic acid (0.2 mmol), ethanol (2 ml), H2O (2 ml) and pyridine (0.2 ml), were placed in a Pyrex tube (ca 20 cm). The tube was frozen with liquid N2, evacuated under vacuum, sealed with a torch and heated at 353 K for two days to give orange-red plate crystals (I), with a yield of 85%.
H atoms on C atoms were positioned geometrically and were treated as riding and refined isotropically, with C—H distances of 0.95 Å and Uiso(H) = 1.2eq(C). H atoms bound to water O were located in a difference map and refined isotropically with restraint of O—H = 0.82 Å.
Although the crystal structure of guanidinium 5-benzoyl-4- hydroxybenznesulfonate (sulisobenzone) methanol solvate [C(NH2)3+.(C14H11O3)SO3-. CH3OH] (II) was first reported by Russell and Ward in 1996), there is no study on a metal derivative of the aion.
The title compound (I) consists of [Co(H2O)6]2+, [Co(C5H5N)2(C14H10O6S)2Co]2- and four lattice water molecules; the composition is related to [Co(H2O)6][Co(C7H3NO4)2].2H2O (III) (Shiu et al., 2004). The cation and anion lie on inversion sites. In (I), two cobalt atoms are octahedrally coordinated, with Co1 surrounded by two N atoms of two pyridine ligands, and four O atoms of two sulisobenzone ligands; the Co2 is ligated by six O atoms of water molecules (Fig. 1). The Co1—O bond lengths are shorter than those of (III). The geometric parameters of 5-benzoyl-4-hydroxy-2-methoxybenzenesulfonate are comparable with those of (II) (Russell & Ward, 1996). The methoxyl group is oriented away from the sulfonate group so that the sulfonate group is sterically accessible for hydrogen bonding with cation and the lattice water donors.
The packing is governed by hydrogen bonds involving the aqua ligands, sulfonate groups and lattice water molecules (Fig.2 and Table 2) to give rise to a three-dimensional network motif.
For related literature, see: Russell & Ward (1996); Shiu et al. (2004).
Data collection: CrystalClear (Rigaku, 1999); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku/MSC & Rigaku, 2000); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.
[Co(H2O)6][Co(C14H10O6S)2(C5H5N)2]·4H2O | F(000) = 1108 |
Mr = 1068.78 | Dx = 1.504 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71070 Å |
Hall symbol: -p 2ybc | Cell parameters from 6940 reflections |
a = 20.373 (3) Å | θ = 3.0–25.3° |
b = 7.1181 (9) Å | µ = 0.87 mm−1 |
c = 17.497 (3) Å | T = 193 K |
β = 111.514 (4)° | Platelet, orange |
V = 2360.5 (6) Å3 | 0.32 × 0.21 × 0.06 mm |
Z = 2 |
Rigaku Mercury diffractometer | 4319 independent reflections |
Radiation source: fine-focus sealed tube | 3462 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.058 |
Detector resolution: 7.31 pixels mm-1 | θmax = 25.3°, θmin = 3.1° |
ω scans | h = −23→24 |
Absorption correction: multi-scan (Jacobson, 1998) | k = −8→8 |
Tmin = 0.768, Tmax = 0.950 | l = −20→21 |
22147 measured reflections |
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)] = 0.051 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.103 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.14 | w = 1/[σ2(Fo2) + (0.0304P)2 + 2.5747P] where P = (Fo2 + 2Fc2)/3 |
4319 reflections | (Δ/σ)max < 0.001 |
343 parameters | Δρmax = 0.68 e Å−3 |
13 restraints | Δρmin = −0.38 e Å−3 |
[Co(H2O)6][Co(C14H10O6S)2(C5H5N)2]·4H2O | V = 2360.5 (6) Å3 |
Mr = 1068.78 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 20.373 (3) Å | µ = 0.87 mm−1 |
b = 7.1181 (9) Å | T = 193 K |
c = 17.497 (3) Å | 0.32 × 0.21 × 0.06 mm |
β = 111.514 (4)° |
Rigaku Mercury diffractometer | 4319 independent reflections |
Absorption correction: multi-scan (Jacobson, 1998) | 3462 reflections with I > 2σ(I) |
Tmin = 0.768, Tmax = 0.950 | Rint = 0.058 |
22147 measured reflections |
R[F2 > 2σ(F2)] = 0.051 | 13 restraints |
wR(F2) = 0.103 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.14 | Δρmax = 0.68 e Å−3 |
4319 reflections | Δρmin = −0.38 e Å−3 |
343 parameters |
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Co1 | 0.5000 | 0.5000 | 0.5000 | 0.02003 (16) | |
Co2 | 0.0000 | 0.5000 | 0.0000 | 0.02028 (16) | |
S1 | 0.12304 (4) | 0.49322 (11) | 0.41394 (4) | 0.01826 (18) | |
O1 | 0.42104 (11) | 0.6814 (3) | 0.48558 (13) | 0.0250 (5) | |
O2 | 0.42779 (11) | 0.3420 (3) | 0.40685 (13) | 0.0244 (5) | |
O3 | 0.19800 (11) | 0.8273 (3) | 0.49728 (14) | 0.0281 (5) | |
O4 | 0.11333 (11) | 0.4893 (3) | 0.49252 (12) | 0.0241 (5) | |
O5 | 0.11111 (11) | 0.3096 (3) | 0.37406 (13) | 0.0248 (5) | |
O6 | 0.08083 (11) | 0.6411 (3) | 0.36010 (13) | 0.0259 (5) | |
O7 | −0.04346 (13) | 0.4972 (4) | 0.09263 (15) | 0.0278 (5) | |
H7A | −0.062 (2) | 0.402 (4) | 0.102 (3) | 0.056 (14)* | |
H7B | −0.0636 (18) | 0.593 (3) | 0.098 (2) | 0.038 (12)* | |
O8 | 0.06503 (16) | 0.7105 (4) | 0.06326 (16) | 0.0422 (7) | |
H8A | 0.078 (2) | 0.726 (7) | 0.1136 (8) | 0.071 (16)* | |
H8B | 0.080 (2) | 0.796 (4) | 0.042 (2) | 0.053 (14)* | |
O9 | 0.07215 (14) | 0.3021 (4) | 0.06926 (16) | 0.0334 (6) | |
H9A | 0.071 (3) | 0.273 (7) | 0.1146 (16) | 0.084 (18)* | |
H9B | 0.080 (3) | 0.207 (4) | 0.047 (3) | 0.088 (19)* | |
O10 | 0.06752 (15) | 0.1624 (4) | 0.21393 (16) | 0.0382 (6) | |
H10A | 0.081 (2) | 0.232 (5) | 0.2539 (17) | 0.059 (15)* | |
H10B | 0.0248 (7) | 0.146 (7) | 0.200 (3) | 0.077 (18)* | |
O11 | 0.1141 (2) | 0.7821 (6) | 0.22309 (19) | 0.0633 (9) | |
H11A | 0.101 (4) | 0.892 (3) | 0.2191 (18) | 0.25 (5)* | |
H11B | 0.104 (4) | 0.724 (5) | 0.258 (2) | 0.14 (3)* | |
N1 | 0.53214 (13) | 0.6648 (4) | 0.41518 (16) | 0.0246 (6) | |
C1 | 0.35542 (16) | 0.6346 (4) | 0.46664 (18) | 0.0205 (7) | |
C2 | 0.31166 (16) | 0.7572 (5) | 0.49088 (19) | 0.0216 (7) | |
H2 | 0.3311 | 0.8703 | 0.5189 | 0.026* | |
C3 | 0.24190 (16) | 0.7166 (4) | 0.47481 (19) | 0.0217 (7) | |
C4 | 0.21184 (16) | 0.5472 (4) | 0.43321 (19) | 0.0198 (7) | |
C5 | 0.25249 (16) | 0.4312 (4) | 0.40683 (18) | 0.0199 (7) | |
H5 | 0.2317 | 0.3202 | 0.3779 | 0.024* | |
C6 | 0.32401 (15) | 0.4683 (4) | 0.42047 (18) | 0.0198 (7) | |
C7 | 0.36210 (16) | 0.3416 (4) | 0.38757 (18) | 0.0195 (7) | |
C8 | 0.32306 (15) | 0.1984 (5) | 0.32385 (18) | 0.0201 (7) | |
C9 | 0.34515 (17) | 0.0129 (5) | 0.3360 (2) | 0.0265 (7) | |
H9C | 0.3817 | −0.0236 | 0.3857 | 0.032* | |
C10 | 0.3137 (2) | −0.1189 (5) | 0.2755 (2) | 0.0370 (9) | |
H10 | 0.3278 | −0.2467 | 0.2847 | 0.044* | |
C11 | 0.2619 (2) | −0.0669 (6) | 0.2019 (2) | 0.0398 (10) | |
H11 | 0.2415 | −0.1575 | 0.1600 | 0.048* | |
C12 | 0.24051 (19) | 0.1172 (6) | 0.1902 (2) | 0.0348 (9) | |
H12 | 0.2050 | 0.1535 | 0.1397 | 0.042* | |
C13 | 0.26956 (17) | 0.2501 (5) | 0.25025 (19) | 0.0276 (8) | |
H13 | 0.2533 | 0.3763 | 0.2417 | 0.033* | |
C14 | 0.22528 (18) | 0.9989 (5) | 0.5402 (2) | 0.0344 (9) | |
H14A | 0.2663 | 0.9712 | 0.5899 | 0.052* | |
H14B | 0.1888 | 1.0599 | 0.5555 | 0.052* | |
H14C | 0.2394 | 1.0828 | 0.5046 | 0.052* | |
C15 | 0.52623 (18) | 0.8529 (5) | 0.4150 (2) | 0.0308 (8) | |
H15 | 0.5084 | 0.9089 | 0.4527 | 0.037* | |
C16 | 0.5445 (2) | 0.9684 (5) | 0.3632 (2) | 0.0377 (9) | |
H16 | 0.5387 | 1.1006 | 0.3645 | 0.045* | |
C17 | 0.5716 (2) | 0.8887 (6) | 0.3094 (2) | 0.0422 (10) | |
H17 | 0.5847 | 0.9649 | 0.2728 | 0.051* | |
C18 | 0.5793 (2) | 0.6978 (6) | 0.3096 (2) | 0.0397 (9) | |
H18 | 0.5987 | 0.6395 | 0.2738 | 0.048* | |
C19 | 0.55858 (18) | 0.5911 (5) | 0.3625 (2) | 0.0312 (8) | |
H19 | 0.5633 | 0.4585 | 0.3614 | 0.037* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0128 (3) | 0.0263 (3) | 0.0220 (3) | −0.0002 (3) | 0.0076 (2) | −0.0032 (3) |
Co2 | 0.0220 (3) | 0.0177 (3) | 0.0250 (3) | −0.0001 (3) | 0.0131 (3) | 0.0001 (3) |
S1 | 0.0163 (4) | 0.0187 (4) | 0.0218 (4) | −0.0006 (3) | 0.0093 (3) | −0.0008 (3) |
O1 | 0.0154 (11) | 0.0268 (13) | 0.0335 (13) | −0.0009 (10) | 0.0100 (10) | −0.0030 (10) |
O2 | 0.0169 (12) | 0.0304 (13) | 0.0272 (12) | 0.0007 (10) | 0.0096 (10) | −0.0061 (10) |
O3 | 0.0200 (12) | 0.0248 (13) | 0.0423 (14) | 0.0001 (10) | 0.0147 (11) | −0.0123 (11) |
O4 | 0.0276 (12) | 0.0257 (12) | 0.0252 (11) | −0.0012 (10) | 0.0168 (10) | 0.0003 (10) |
O5 | 0.0243 (12) | 0.0232 (12) | 0.0299 (12) | −0.0051 (10) | 0.0134 (10) | −0.0072 (10) |
O6 | 0.0212 (12) | 0.0258 (13) | 0.0294 (12) | 0.0039 (10) | 0.0077 (10) | 0.0027 (10) |
O7 | 0.0351 (14) | 0.0200 (13) | 0.0384 (13) | 0.0014 (13) | 0.0253 (12) | 0.0017 (12) |
O8 | 0.0600 (19) | 0.0413 (17) | 0.0288 (15) | −0.0267 (15) | 0.0203 (14) | −0.0054 (13) |
O9 | 0.0402 (15) | 0.0336 (15) | 0.0313 (14) | 0.0141 (13) | 0.0190 (13) | 0.0047 (13) |
O10 | 0.0318 (16) | 0.0519 (19) | 0.0294 (15) | −0.0063 (14) | 0.0094 (13) | −0.0052 (13) |
O11 | 0.091 (3) | 0.064 (2) | 0.0414 (18) | −0.018 (2) | 0.0311 (18) | 0.0007 (16) |
N1 | 0.0212 (14) | 0.0286 (16) | 0.0254 (14) | 0.0004 (12) | 0.0101 (12) | −0.0028 (13) |
C1 | 0.0177 (16) | 0.0216 (17) | 0.0234 (16) | −0.0011 (13) | 0.0092 (14) | 0.0019 (14) |
C2 | 0.0188 (16) | 0.0198 (17) | 0.0267 (17) | −0.0010 (13) | 0.0087 (14) | −0.0043 (14) |
C3 | 0.0201 (16) | 0.0210 (18) | 0.0274 (17) | 0.0035 (14) | 0.0128 (14) | 0.0000 (14) |
C4 | 0.0159 (15) | 0.0196 (17) | 0.0254 (16) | −0.0012 (13) | 0.0093 (14) | 0.0008 (13) |
C5 | 0.0181 (16) | 0.0193 (16) | 0.0215 (16) | 0.0008 (13) | 0.0066 (14) | −0.0008 (13) |
C6 | 0.0150 (15) | 0.0236 (18) | 0.0204 (15) | 0.0007 (13) | 0.0061 (13) | 0.0000 (13) |
C7 | 0.0186 (16) | 0.0210 (17) | 0.0202 (16) | 0.0026 (13) | 0.0088 (13) | 0.0038 (13) |
C8 | 0.0171 (16) | 0.0263 (18) | 0.0208 (16) | −0.0003 (14) | 0.0113 (14) | −0.0009 (14) |
C9 | 0.0245 (17) | 0.0262 (19) | 0.0278 (17) | 0.0015 (15) | 0.0086 (15) | 0.0022 (15) |
C10 | 0.045 (2) | 0.024 (2) | 0.045 (2) | −0.0031 (17) | 0.020 (2) | −0.0050 (17) |
C11 | 0.041 (2) | 0.039 (2) | 0.039 (2) | −0.0124 (19) | 0.014 (2) | −0.0161 (19) |
C12 | 0.0287 (19) | 0.045 (2) | 0.0264 (19) | −0.0027 (18) | 0.0049 (16) | −0.0053 (17) |
C13 | 0.0230 (18) | 0.0299 (19) | 0.0282 (18) | 0.0039 (15) | 0.0075 (15) | −0.0001 (15) |
C14 | 0.0285 (19) | 0.0266 (19) | 0.050 (2) | 0.0001 (17) | 0.0167 (17) | −0.0184 (18) |
C15 | 0.0291 (19) | 0.030 (2) | 0.0333 (19) | 0.0034 (16) | 0.0118 (16) | −0.0031 (16) |
C16 | 0.038 (2) | 0.029 (2) | 0.042 (2) | −0.0036 (17) | 0.0113 (19) | 0.0038 (18) |
C17 | 0.039 (2) | 0.050 (3) | 0.042 (2) | −0.007 (2) | 0.0193 (19) | 0.012 (2) |
C18 | 0.040 (2) | 0.049 (3) | 0.040 (2) | −0.0003 (19) | 0.0261 (19) | 0.0011 (19) |
C19 | 0.034 (2) | 0.031 (2) | 0.0322 (19) | 0.0018 (17) | 0.0172 (17) | −0.0017 (16) |
Co1—O1i | 2.005 (2) | C1—C6 | 1.443 (4) |
Co1—O1 | 2.005 (2) | C2—C3 | 1.375 (4) |
Co1—O2i | 2.080 (2) | C2—H2 | 0.9500 |
Co1—O2 | 2.080 (2) | C3—C4 | 1.426 (4) |
Co1—N1i | 2.173 (3) | C4—C5 | 1.364 (4) |
Co1—N1 | 2.173 (3) | C5—C6 | 1.412 (4) |
Co2—O7 | 2.113 (2) | C5—H5 | 0.9500 |
Co2—O8 | 2.037 (3) | C6—C7 | 1.440 (4) |
Co2—O8ii | 2.037 (3) | C7—C8 | 1.505 (4) |
Co2—O9 | 2.075 (3) | C8—C9 | 1.386 (5) |
Co2—O9ii | 2.075 (3) | C8—C13 | 1.397 (4) |
Co2—O7ii | 2.113 (2) | C9—C10 | 1.383 (5) |
S1—O5 | 1.459 (2) | C9—H9C | 0.9500 |
S1—O4 | 1.459 (2) | C10—C11 | 1.382 (5) |
S1—O6 | 1.463 (2) | C10—H10 | 0.9500 |
S1—C4 | 1.757 (3) | C11—C12 | 1.373 (5) |
O1—C1 | 1.297 (4) | C11—H11 | 0.9500 |
C7—O2 | 1.254 (4) | C12—C13 | 1.376 (5) |
O3—C3 | 1.354 (4) | C12—H12 | 0.9500 |
O3—C14 | 1.435 (4) | C13—H13 | 0.9500 |
O7—H7A | 0.82 (3) | C14—H14A | 0.9800 |
O7—H7B | 0.82 (3) | C14—H14B | 0.9800 |
O8—H8A | 0.829 (10) | C14—H14C | 0.9800 |
O8—H8B | 0.83 (3) | C15—C16 | 1.372 (5) |
O9—H9A | 0.83 (3) | C15—H15 | 0.9500 |
O9—H9B | 0.83 (4) | C16—C17 | 1.376 (5) |
O10—H10A | 0.82 (3) | C16—H16 | 0.9500 |
O10—H10B | 0.82 (3) | C17—C18 | 1.368 (6) |
O11—H11A | 0.82 (3) | C17—H17 | 0.9500 |
O11—H11B | 0.82 (5) | C18—C19 | 1.378 (5) |
N1—C19 | 1.333 (4) | C18—H18 | 0.9500 |
N1—C15 | 1.344 (4) | C19—H19 | 0.9500 |
C1—C2 | 1.419 (4) | ||
O1i—Co1—O1 | 180.00 (13) | C3—C2—H2 | 119.2 |
O1i—Co1—O2i | 86.87 (9) | C1—C2—H2 | 119.2 |
O1—Co1—O2i | 93.13 (9) | O3—C3—C2 | 124.2 (3) |
O1i—Co1—O2 | 93.13 (9) | O3—C3—C4 | 115.8 (3) |
O1—Co1—O2 | 86.87 (9) | C2—C3—C4 | 120.1 (3) |
O2i—Co1—O2 | 180.0 | C5—C4—C3 | 119.0 (3) |
O1i—Co1—N1i | 89.72 (9) | C5—C4—S1 | 120.9 (2) |
O1—Co1—N1i | 90.28 (9) | C3—C4—S1 | 120.1 (2) |
O2i—Co1—N1i | 93.47 (9) | C4—C5—C6 | 123.1 (3) |
O2—Co1—N1i | 86.53 (9) | C4—C5—H5 | 118.4 |
O1i—Co1—N1 | 90.28 (9) | C6—C5—H5 | 118.4 |
O1—Co1—N1 | 89.72 (9) | C5—C6—C7 | 119.3 (3) |
O2i—Co1—N1 | 86.53 (9) | C5—C6—C1 | 117.8 (3) |
O2—Co1—N1 | 93.47 (9) | C7—C6—C1 | 122.9 (3) |
N1i—Co1—N1 | 180.0 | O2—C7—C6 | 124.7 (3) |
O7—Co2—O8 | 87.83 (10) | O2—C7—C8 | 115.0 (3) |
O7—Co2—O9 | 87.25 (10) | C6—C7—C8 | 120.3 (3) |
O8—Co2—O8ii | 180.0 (3) | C9—C8—C13 | 119.5 (3) |
O8—Co2—O9 | 90.10 (12) | C9—C8—C7 | 118.5 (3) |
O8ii—Co2—O9 | 89.90 (12) | C13—C8—C7 | 121.7 (3) |
O8—Co2—O9ii | 89.90 (12) | C10—C9—C8 | 119.7 (3) |
O8ii—Co2—O9ii | 90.10 (12) | C10—C9—H9C | 120.2 |
O9—Co2—O9ii | 180.0 (2) | C8—C9—H9C | 120.2 |
O8—Co2—O7ii | 92.17 (10) | C11—C10—C9 | 120.9 (4) |
O8ii—Co2—O7ii | 87.83 (10) | C11—C10—H10 | 119.6 |
O9—Co2—O7ii | 92.75 (10) | C9—C10—H10 | 119.6 |
O9ii—Co2—O7ii | 87.25 (10) | C12—C11—C10 | 119.1 (3) |
O8ii—Co2—O7 | 92.17 (10) | C12—C11—H11 | 120.4 |
O9ii—Co2—O7 | 92.75 (10) | C10—C11—H11 | 120.4 |
O7ii—Co2—O7 | 180.00 (9) | C11—C12—C13 | 121.2 (3) |
O5—S1—O4 | 112.16 (13) | C11—C12—H12 | 119.4 |
O5—S1—O6 | 112.40 (13) | C13—C12—H12 | 119.4 |
O4—S1—O6 | 111.69 (13) | C12—C13—C8 | 119.6 (3) |
O5—S1—C4 | 105.46 (14) | C12—C13—H13 | 120.2 |
O4—S1—C4 | 108.01 (14) | C8—C13—H13 | 120.2 |
O6—S1—C4 | 106.67 (14) | O3—C14—H14A | 109.5 |
C1—O1—Co1 | 124.8 (2) | O3—C14—H14B | 109.5 |
C7—O2—Co1 | 126.2 (2) | H14A—C14—H14B | 109.5 |
C3—O3—C14 | 118.5 (2) | O3—C14—H14C | 109.5 |
Co2—O7—H7A | 121 (3) | H14A—C14—H14C | 109.5 |
Co2—O7—H7B | 117 (3) | H14B—C14—H14C | 109.5 |
H7A—O7—H7B | 112 (4) | N1—C15—C16 | 123.6 (3) |
Co2—O8—H8A | 124 (3) | N1—C15—H15 | 118.2 |
Co2—O8—H8B | 125 (3) | C16—C15—H15 | 118.2 |
H8A—O8—H8B | 111 (4) | C15—C16—C17 | 118.6 (4) |
Co2—O9—H9A | 118 (4) | C15—C16—H16 | 120.7 |
Co2—O9—H9B | 119 (4) | C17—C16—H16 | 120.7 |
H9A—O9—H9B | 109 (5) | C18—C17—C16 | 118.8 (4) |
H10A—O10—H10B | 109 (5) | C18—C17—H17 | 120.6 |
H11A—O11—H11B | 112 (6) | C16—C17—H17 | 120.6 |
C19—N1—C15 | 116.6 (3) | C17—C18—C19 | 119.1 (4) |
C19—N1—Co1 | 124.0 (2) | C17—C18—H18 | 120.5 |
C15—N1—Co1 | 119.4 (2) | C19—C18—H18 | 120.5 |
O1—C1—C2 | 117.8 (3) | N1—C19—C18 | 123.3 (4) |
O1—C1—C6 | 123.9 (3) | N1—C19—H19 | 118.4 |
C2—C1—C6 | 118.3 (3) | C18—C19—H19 | 118.4 |
C3—C2—C1 | 121.7 (3) | ||
O2i—Co1—O1—C1 | −145.3 (2) | C3—C4—C5—C6 | 1.6 (5) |
O2—Co1—O1—C1 | 34.7 (2) | S1—C4—C5—C6 | 179.8 (2) |
N1i—Co1—O1—C1 | −51.8 (2) | C4—C5—C6—C7 | −177.6 (3) |
N1—Co1—O1—C1 | 128.2 (2) | C4—C5—C6—C1 | 1.8 (5) |
O1i—Co1—O2—C7 | 154.5 (3) | O1—C1—C6—C5 | 177.8 (3) |
O1—Co1—O2—C7 | −25.5 (3) | C2—C1—C6—C5 | −4.1 (4) |
N1i—Co1—O2—C7 | 65.0 (3) | O1—C1—C6—C7 | −2.8 (5) |
N1—Co1—O2—C7 | −115.0 (3) | C2—C1—C6—C7 | 175.3 (3) |
O1i—Co1—N1—C19 | 35.2 (3) | Co1—O2—C7—C6 | 7.8 (4) |
O1—Co1—N1—C19 | −144.8 (3) | Co1—O2—C7—C8 | −173.65 (19) |
O2i—Co1—N1—C19 | 122.0 (3) | C5—C6—C7—O2 | −167.5 (3) |
O2—Co1—N1—C19 | −58.0 (3) | C1—C6—C7—O2 | 13.1 (5) |
O1i—Co1—N1—C15 | −144.2 (2) | C5—C6—C7—C8 | 14.0 (4) |
O1—Co1—N1—C15 | 35.8 (2) | C1—C6—C7—C8 | −165.4 (3) |
O2i—Co1—N1—C15 | −57.3 (2) | O2—C7—C8—C9 | 51.5 (4) |
O2—Co1—N1—C15 | 122.7 (2) | C6—C7—C8—C9 | −129.8 (3) |
Co1—O1—C1—C2 | 154.4 (2) | O2—C7—C8—C13 | −123.0 (3) |
Co1—O1—C1—C6 | −27.5 (4) | C6—C7—C8—C13 | 55.6 (4) |
O1—C1—C2—C3 | −178.7 (3) | C13—C8—C9—C10 | −0.4 (5) |
C6—C1—C2—C3 | 3.1 (5) | C7—C8—C9—C10 | −175.1 (3) |
C14—O3—C3—C2 | 0.4 (5) | C8—C9—C10—C11 | 2.0 (5) |
C14—O3—C3—C4 | 179.3 (3) | C9—C10—C11—C12 | −1.8 (6) |
C1—C2—C3—O3 | 179.2 (3) | C10—C11—C12—C13 | 0.0 (6) |
C1—C2—C3—C4 | 0.4 (5) | C11—C12—C13—C8 | 1.6 (5) |
O3—C3—C4—C5 | 178.3 (3) | C9—C8—C13—C12 | −1.3 (5) |
C2—C3—C4—C5 | −2.8 (5) | C7—C8—C13—C12 | 173.1 (3) |
O3—C3—C4—S1 | 0.1 (4) | C19—N1—C15—C16 | 1.2 (5) |
C2—C3—C4—S1 | 179.1 (2) | Co1—N1—C15—C16 | −179.4 (3) |
O5—S1—C4—C5 | 4.0 (3) | N1—C15—C16—C17 | −1.2 (6) |
O4—S1—C4—C5 | 124.1 (3) | C15—C16—C17—C18 | −0.1 (6) |
O6—S1—C4—C5 | −115.7 (3) | C16—C17—C18—C19 | 1.2 (6) |
O5—S1—C4—C3 | −177.8 (2) | C15—N1—C19—C18 | 0.0 (5) |
O4—S1—C4—C3 | −57.8 (3) | Co1—N1—C19—C18 | −179.4 (3) |
O6—S1—C4—C3 | 62.4 (3) | C17—C18—C19—N1 | −1.2 (6) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x, −y+1, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7A···O6iii | 0.82 (3) | 2.06 (2) | 2.855 (3) | 164 (4) |
O7—H7B···O5iv | 0.82 (3) | 1.98 (3) | 2.788 (3) | 172 (4) |
O8—H8A···O11 | 0.83 (1) | 1.83 (1) | 2.651 (4) | 173 (5) |
O8—H8B···O4v | 0.82 (3) | 1.99 (3) | 2.821 (3) | 178 (4) |
O9—H9A···O10 | 0.83 (3) | 1.93 (4) | 2.753 (4) | 170 (5) |
O9—H9B···O4vi | 0.83 (4) | 1.95 (5) | 2.763 (3) | 169 (5) |
O10—H10A···O5 | 0.82 (3) | 2.04 (2) | 2.813 (3) | 158 (4) |
O10—H10B···O6iii | 0.82 (3) | 2.02 (2) | 2.822 (3) | 166 (5) |
O11—H11A···O10vii | 0.82 (3) | 2.03 (3) | 2.853 (5) | 177 (5) |
O11—H11B···O6 | 0.82 (5) | 2.09 (5) | 2.899 (4) | 166 (4) |
Symmetry codes: (iii) −x, y−1/2, −z+1/2; (iv) −x, y+1/2, −z+1/2; (v) x, −y+3/2, z−1/2; (vi) x, −y+1/2, z−1/2; (vii) x, y+1, z. |
Experimental details
Crystal data | |
Chemical formula | [Co(H2O)6][Co(C14H10O6S)2(C5H5N)2]·4H2O |
Mr | 1068.78 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 193 |
a, b, c (Å) | 20.373 (3), 7.1181 (9), 17.497 (3) |
β (°) | 111.514 (4) |
V (Å3) | 2360.5 (6) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.87 |
Crystal size (mm) | 0.32 × 0.21 × 0.06 |
Data collection | |
Diffractometer | Rigaku Mercury |
Absorption correction | Multi-scan (Jacobson, 1998) |
Tmin, Tmax | 0.768, 0.950 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 22147, 4319, 3462 |
Rint | 0.058 |
(sin θ/λ)max (Å−1) | 0.602 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.051, 0.103, 1.14 |
No. of reflections | 4319 |
No. of parameters | 343 |
No. of restraints | 13 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.68, −0.38 |
Computer programs: CrystalClear (Rigaku, 1999), CrystalClear, CrystalStructure (Rigaku/MSC & Rigaku, 2000), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 1997), SHELXTL.
Co1—O1 | 2.005 (2) | Co2—O8 | 2.037 (3) |
Co1—O2 | 2.080 (2) | Co2—O9 | 2.075 (3) |
Co1—N1 | 2.173 (3) | C7—O2 | 1.254 (4) |
Co2—O7 | 2.113 (2) | ||
O1i—Co1—O1 | 180.00 (13) | N1i—Co1—N1 | 180.0 |
O1—Co1—O2 | 86.87 (9) | O7—Co2—O8 | 87.83 (10) |
O1—Co1—N1i | 90.28 (9) | O7—Co2—O9 | 87.25 (10) |
O1—Co1—N1 | 89.72 (9) | O8—Co2—O9 | 90.10 (12) |
O2—Co1—N1 | 93.47 (9) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7A···O6ii | 0.82 (3) | 2.059 (16) | 2.855 (3) | 164 (4) |
O7—H7B···O5iii | 0.82 (3) | 1.98 (3) | 2.788 (3) | 172 (4) |
O8—H8A···O11 | 0.829 (10) | 1.827 (13) | 2.651 (4) | 173 (5) |
O8—H8B···O4iv | 0.82 (3) | 1.99 (3) | 2.821 (3) | 178 (4) |
O9—H9A···O10 | 0.83 (3) | 1.93 (4) | 2.753 (4) | 170 (5) |
O9—H9B···O4v | 0.83 (4) | 1.95 (5) | 2.763 (3) | 169 (5) |
O10—H10A···O5 | 0.82 (3) | 2.04 (2) | 2.813 (3) | 158 (4) |
O10—H10B···O6ii | 0.82 (3) | 2.019 (16) | 2.822 (3) | 166 (5) |
O11—H11A···O10vi | 0.82 (3) | 2.03 (3) | 2.853 (5) | 177 (5) |
O11—H11B···O6 | 0.82 (5) | 2.09 (5) | 2.899 (4) | 166 (4) |
Symmetry codes: (ii) −x, y−1/2, −z+1/2; (iii) −x, y+1/2, −z+1/2; (iv) x, −y+3/2, z−1/2; (v) x, −y+1/2, z−1/2; (vi) x, y+1, z. |
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Although the crystal structure of guanidinium 5-benzoyl-4- hydroxybenznesulfonate (sulisobenzone) methanol solvate [C(NH2)3+.(C14H11O3)SO3-. CH3OH] (II) was first reported by Russell and Ward in 1996), there is no study on a metal derivative of the aion.
The title compound (I) consists of [Co(H2O)6]2+, [Co(C5H5N)2(C14H10O6S)2Co]2- and four lattice water molecules; the composition is related to [Co(H2O)6][Co(C7H3NO4)2].2H2O (III) (Shiu et al., 2004). The cation and anion lie on inversion sites. In (I), two cobalt atoms are octahedrally coordinated, with Co1 surrounded by two N atoms of two pyridine ligands, and four O atoms of two sulisobenzone ligands; the Co2 is ligated by six O atoms of water molecules (Fig. 1). The Co1—O bond lengths are shorter than those of (III). The geometric parameters of 5-benzoyl-4-hydroxy-2-methoxybenzenesulfonate are comparable with those of (II) (Russell & Ward, 1996). The methoxyl group is oriented away from the sulfonate group so that the sulfonate group is sterically accessible for hydrogen bonding with cation and the lattice water donors.
The packing is governed by hydrogen bonds involving the aqua ligands, sulfonate groups and lattice water molecules (Fig.2 and Table 2) to give rise to a three-dimensional network motif.