Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270103026957/bm1550sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270103026957/bm1550Isup2.hkl |
CCDC reference: 231040
To a solution of CoCl2·6H2O (0.2379 g, 1.00 mmol) was added 4-aminobenzenesulfonic acid (0.074 g, 0.54 mmol) with stirring. ##AUTHOR: Give temperature used for the above reaction. After the solution pH had been adjusted to ca 5.5 with dilute NaOH, 1,10-phen (0.078 g, 0.50 mmol) was added slowly and the mixture was stirred for 30 min at 333 K. After filtration, a clear orange solution was obtained, which was allowed to stand at room temperatur. Orange crystals were obtained after two weeks.
An 8% decay correction was applied to the data during processing. Water H atoms were located from difference maps and their positions were fixed during refinement. Other H atoms were placed in geometric positions using a riding model, with C—H distances of 0.93 Å and N—H distances of 0.90 Å [Uiso(H) = 1.2 Ueq(C)].
Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Co(C6H6NO3S)(C12H8N2)(H2O)3]Cl | F(000) = 1028 |
Mr = 500.81 | Dx = 1.616 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 7.0148 (10) Å | Cell parameters from 24 reflections |
b = 15.896 (4) Å | θ = 5.2–10.2° |
c = 18.587 (5) Å | µ = 1.11 mm−1 |
β = 96.548 (18)° | T = 293 K |
V = 2059.0 (8) Å3 | Block, orange |
Z = 4 | 0.50 × 0.38 × 0.32 mm |
Siemens P4 diffractometer | 2959 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.026 |
Graphite monochromator | θmax = 26.0°, θmin = 1.7° |
ω scans | h = −1→8 |
Absorption correction: ψ scan (SHELXTL; Siemens, 1994) | k = −1→19 |
Tmin = 0.561, Tmax = 0.687 | l = −22→22 |
5562 measured reflections | 3 standard reflections every 97 reflections |
4060 independent reflections | intensity decay: 8.0% |
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)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.073 | H-atom parameters constrained |
S = 1.09 | w = 1/[σ2(Fo2) + (0.02P)2] where P = (Fo2 + 2Fc2)/3 |
4060 reflections | (Δ/σ)max = 0.001 |
271 parameters | Δρmax = 0.31 e Å−3 |
0 restraints | Δρmin = −0.37 e Å−3 |
[Co(C6H6NO3S)(C12H8N2)(H2O)3]Cl | V = 2059.0 (8) Å3 |
Mr = 500.81 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 7.0148 (10) Å | µ = 1.11 mm−1 |
b = 15.896 (4) Å | T = 293 K |
c = 18.587 (5) Å | 0.50 × 0.38 × 0.32 mm |
β = 96.548 (18)° |
Siemens P4 diffractometer | 2959 reflections with I > 2σ(I) |
Absorption correction: ψ scan (SHELXTL; Siemens, 1994) | Rint = 0.026 |
Tmin = 0.561, Tmax = 0.687 | 3 standard reflections every 97 reflections |
5562 measured reflections | intensity decay: 8.0% |
4060 independent reflections |
R[F2 > 2σ(F2)] = 0.034 | 0 restraints |
wR(F2) = 0.073 | H-atom parameters constrained |
S = 1.09 | Δρmax = 0.31 e Å−3 |
4060 reflections | Δρmin = −0.37 e Å−3 |
271 parameters |
x | y | z | Uiso*/Ueq | ||
Co | 0.18360 (6) | 0.18776 (2) | 0.42688 (2) | 0.0273 (1) | |
S | −0.16070 (10) | 0.48381 (4) | 0.14583 (3) | 0.0277 (2) | |
O1 | −0.0033 (3) | 0.46813 (11) | 0.10247 (10) | 0.0387 (7) | |
OW1 | 0.0349 (3) | 0.15217 (13) | 0.51162 (11) | 0.0521 (8) | |
O2 | −0.3478 (3) | 0.47139 (11) | 0.10292 (9) | 0.0350 (6) | |
OW2 | 0.4412 (3) | 0.14893 (11) | 0.48404 (10) | 0.0437 (7) | |
O3 | −0.1511 (3) | 0.56343 (10) | 0.18319 (9) | 0.0398 (6) | |
OW3 | 0.1668 (3) | 0.06711 (11) | 0.38174 (10) | 0.0366 (6) | |
N1 | 0.3058 (3) | 0.24285 (13) | 0.33898 (11) | 0.0283 (7) | |
N2 | 0.2252 (3) | 0.31366 (13) | 0.46217 (11) | 0.0292 (7) | |
N3 | −0.1159 (3) | 0.21745 (13) | 0.37323 (11) | 0.0311 (7) | |
C1 | 0.3422 (4) | 0.20688 (17) | 0.27748 (14) | 0.0359 (9) | |
C2 | 0.3801 (5) | 0.2534 (2) | 0.21722 (15) | 0.0443 (10) | |
C3 | 0.3821 (4) | 0.33875 (19) | 0.22010 (15) | 0.0423 (10) | |
C4 | 0.3509 (4) | 0.37970 (18) | 0.28475 (15) | 0.0356 (9) | |
C5 | 0.3116 (4) | 0.32830 (15) | 0.34274 (14) | 0.0276 (8) | |
C6 | 0.2756 (4) | 0.36596 (15) | 0.40964 (14) | 0.0290 (8) | |
C7 | 0.2905 (4) | 0.45374 (16) | 0.41875 (16) | 0.0371 (9) | |
C8 | 0.2583 (5) | 0.48595 (18) | 0.48658 (17) | 0.0475 (11) | |
C9 | 0.2159 (5) | 0.43275 (19) | 0.53929 (16) | 0.0468 (10) | |
C10 | 0.1983 (4) | 0.34738 (17) | 0.52587 (14) | 0.0372 (9) | |
C11 | 0.3577 (5) | 0.46915 (18) | 0.29430 (17) | 0.0460 (11) | |
C12 | 0.3299 (5) | 0.50389 (17) | 0.35808 (18) | 0.0473 (11) | |
C13 | −0.1362 (4) | 0.28042 (16) | 0.31810 (13) | 0.0282 (8) | |
C14 | −0.1596 (4) | 0.36385 (16) | 0.33630 (13) | 0.0314 (9) | |
C15 | −0.1645 (4) | 0.42566 (15) | 0.28423 (13) | 0.0307 (9) | |
C16 | −0.1458 (4) | 0.40461 (14) | 0.21292 (13) | 0.0262 (8) | |
C17 | −0.1216 (4) | 0.32105 (15) | 0.19419 (13) | 0.0306 (8) | |
C18 | −0.1182 (4) | 0.25938 (15) | 0.24649 (14) | 0.0315 (8) | |
Cl | 0.22774 (12) | 0.21391 (4) | 0.02904 (4) | 0.0433 (2) | |
H1 | 0.34230 | 0.14850 | 0.27450 | 0.0430* | |
HW1 | 0.07190 | 0.11440 | 0.54180 | 0.0630* | |
H2 | 0.40410 | 0.22600 | 0.17500 | 0.0530* | |
HW2 | −0.07260 | 0.18240 | 0.52550 | 0.0630* | |
H3 | 0.40400 | 0.36990 | 0.17950 | 0.0510* | |
HW3 | 0.52740 | 0.19310 | 0.50390 | 0.0520* | |
H3A | −0.16690 | 0.16950 | 0.35390 | 0.0370* | |
H3B | −0.18750 | 0.23320 | 0.40820 | 0.0370* | |
HW4 | 0.45280 | 0.10360 | 0.51280 | 0.0520* | |
HW5 | 0.05590 | 0.03880 | 0.38600 | 0.0440* | |
HW6 | 0.28190 | 0.03790 | 0.39200 | 0.0440* | |
H8 | 0.26600 | 0.54350 | 0.49530 | 0.0570* | |
H9 | 0.19850 | 0.45370 | 0.58480 | 0.0560* | |
H10 | 0.16660 | 0.31220 | 0.56270 | 0.0450* | |
H11 | 0.38150 | 0.50350 | 0.25580 | 0.0550* | |
H12 | 0.33650 | 0.56210 | 0.36310 | 0.0570* | |
H14 | −0.17210 | 0.37830 | 0.38400 | 0.0380* | |
H15 | −0.18040 | 0.48160 | 0.29690 | 0.0370* | |
H17 | −0.10770 | 0.30670 | 0.14660 | 0.0370* | |
H18 | −0.10370 | 0.20330 | 0.23380 | 0.0380* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co | 0.0355 (2) | 0.0203 (2) | 0.0257 (2) | −0.0001 (2) | 0.0020 (2) | 0.0024 (2) |
S | 0.0342 (4) | 0.0189 (3) | 0.0289 (3) | −0.0003 (3) | −0.0005 (3) | −0.0001 (3) |
O1 | 0.0407 (13) | 0.0335 (10) | 0.0438 (11) | −0.0029 (10) | 0.0131 (10) | 0.0023 (9) |
OW1 | 0.0613 (16) | 0.0519 (12) | 0.0468 (12) | 0.0231 (12) | 0.0222 (12) | 0.0273 (10) |
O2 | 0.0380 (12) | 0.0289 (9) | 0.0354 (10) | 0.0036 (9) | −0.0075 (9) | −0.0033 (8) |
OW2 | 0.0471 (13) | 0.0306 (10) | 0.0485 (12) | −0.0048 (10) | −0.0153 (11) | 0.0074 (9) |
O3 | 0.0587 (14) | 0.0206 (9) | 0.0378 (10) | −0.0025 (10) | −0.0039 (10) | −0.0031 (8) |
OW3 | 0.0347 (11) | 0.0249 (9) | 0.0501 (11) | 0.0001 (9) | 0.0047 (10) | −0.0039 (8) |
N1 | 0.0293 (13) | 0.0274 (11) | 0.0282 (11) | 0.0020 (10) | 0.0036 (10) | 0.0008 (9) |
N2 | 0.0342 (13) | 0.0252 (10) | 0.0276 (11) | −0.0015 (11) | 0.0011 (10) | −0.0022 (9) |
N3 | 0.0385 (14) | 0.0255 (10) | 0.0282 (11) | −0.0013 (11) | −0.0003 (11) | 0.0035 (9) |
C1 | 0.0365 (17) | 0.0368 (15) | 0.0348 (15) | 0.0055 (14) | 0.0061 (14) | −0.0023 (12) |
C2 | 0.0434 (19) | 0.0610 (19) | 0.0302 (15) | 0.0042 (17) | 0.0115 (14) | −0.0019 (14) |
C3 | 0.0396 (19) | 0.0548 (18) | 0.0337 (15) | −0.0008 (16) | 0.0088 (14) | 0.0159 (14) |
C4 | 0.0274 (16) | 0.0388 (15) | 0.0392 (16) | −0.0007 (13) | −0.0019 (13) | 0.0109 (13) |
C5 | 0.0253 (15) | 0.0239 (13) | 0.0333 (14) | −0.0008 (11) | 0.0021 (12) | 0.0044 (10) |
C6 | 0.0262 (15) | 0.0241 (12) | 0.0355 (14) | −0.0010 (12) | −0.0021 (12) | 0.0025 (11) |
C7 | 0.0359 (17) | 0.0244 (13) | 0.0492 (17) | −0.0008 (13) | −0.0026 (14) | −0.0005 (12) |
C8 | 0.050 (2) | 0.0282 (14) | 0.062 (2) | 0.0002 (15) | −0.0038 (18) | −0.0155 (15) |
C9 | 0.055 (2) | 0.0427 (17) | 0.0423 (16) | −0.0009 (17) | 0.0041 (16) | −0.0181 (14) |
C10 | 0.0420 (18) | 0.0389 (15) | 0.0300 (14) | −0.0016 (14) | 0.0017 (14) | −0.0031 (12) |
C11 | 0.047 (2) | 0.0369 (16) | 0.0535 (19) | −0.0075 (15) | 0.0037 (17) | 0.0214 (15) |
C12 | 0.045 (2) | 0.0240 (14) | 0.071 (2) | −0.0044 (14) | −0.0014 (18) | 0.0084 (14) |
C13 | 0.0269 (15) | 0.0266 (12) | 0.0298 (13) | −0.0026 (12) | −0.0018 (12) | 0.0033 (11) |
C14 | 0.0372 (17) | 0.0310 (14) | 0.0255 (13) | 0.0047 (13) | 0.0017 (13) | −0.0025 (11) |
C15 | 0.0375 (17) | 0.0230 (13) | 0.0312 (14) | 0.0039 (13) | 0.0017 (13) | −0.0046 (11) |
C16 | 0.0292 (15) | 0.0207 (11) | 0.0278 (13) | −0.0005 (11) | −0.0004 (12) | 0.0003 (10) |
C17 | 0.0398 (17) | 0.0268 (13) | 0.0243 (12) | 0.0012 (13) | −0.0006 (12) | −0.0022 (11) |
C18 | 0.0398 (17) | 0.0192 (12) | 0.0340 (14) | 0.0013 (12) | −0.0017 (13) | −0.0033 (11) |
Cl | 0.0453 (5) | 0.0342 (3) | 0.0498 (4) | 0.0008 (3) | 0.0025 (4) | 0.0056 (3) |
Co—OW1 | 2.065 (2) | C4—C11 | 1.433 (4) |
Co—OW2 | 2.083 (2) | C5—C6 | 1.428 (4) |
Co—OW3 | 2.091 (2) | C6—C7 | 1.408 (4) |
Co—N1 | 2.119 (2) | C7—C8 | 1.403 (4) |
Co—N2 | 2.116 (2) | C7—C12 | 1.433 (4) |
Co—N3 | 2.270 (2) | C8—C9 | 1.353 (4) |
S—O1 | 1.461 (2) | C9—C10 | 1.383 (4) |
S—O2 | 1.469 (2) | C11—C12 | 1.342 (5) |
S—O3 | 1.4415 (18) | C13—C18 | 1.392 (4) |
S—C16 | 1.767 (2) | C13—C14 | 1.383 (4) |
OW1—HW1 | 0.8422 | C14—C15 | 1.377 (3) |
OW1—HW2 | 0.9542 | C15—C16 | 1.388 (3) |
OW2—HW3 | 0.9716 | C16—C17 | 1.389 (3) |
OW2—HW4 | 0.8954 | C17—C18 | 1.379 (3) |
OW3—HW6 | 0.9321 | C1—H1 | 0.93 |
OW3—HW5 | 0.9100 | C2—H2 | 0.93 |
N1—C1 | 1.329 (3) | C3—H3 | 0.93 |
N1—C5 | 1.361 (3) | C8—H8 | 0.93 |
N2—C10 | 1.333 (3) | C9—H9 | 0.93 |
N2—C6 | 1.360 (3) | C10—H10 | 0.93 |
N3—C13 | 1.428 (3) | C11—H11 | 0.93 |
N3—H3A | 0.90 | C12—H12 | 0.93 |
N3—H3B | 0.90 | C14—H14 | 0.93 |
C1—C2 | 1.393 (4) | C15—H15 | 0.93 |
C2—C3 | 1.358 (4) | C17—H17 | 0.93 |
C3—C4 | 1.406 (4) | C18—H18 | 0.93 |
C4—C5 | 1.405 (4) | ||
OW1—Co—OW2 | 90.81 (8) | N1—C5—C6 | 117.1 (2) |
OW1—Co—OW3 | 92.55 (8) | C4—C5—C6 | 119.6 (2) |
OW1—Co—N1 | 170.16 (8) | N1—C5—C4 | 123.3 (2) |
OW1—Co—N2 | 94.96 (8) | C5—C6—C7 | 120.1 (2) |
OW1—Co—N3 | 82.49 (8) | N2—C6—C5 | 117.1 (2) |
OW2—Co—OW3 | 86.49 (8) | N2—C6—C7 | 122.8 (2) |
OW2—Co—N1 | 96.43 (8) | C8—C7—C12 | 124.7 (2) |
OW2—Co—N2 | 92.36 (8) | C6—C7—C12 | 118.4 (3) |
OW2—Co—N3 | 172.50 (8) | C6—C7—C8 | 116.9 (3) |
OW3—Co—N1 | 94.52 (8) | C7—C8—C9 | 119.6 (3) |
OW3—Co—N2 | 172.41 (8) | C8—C9—C10 | 120.4 (3) |
OW3—Co—N3 | 90.43 (8) | N2—C10—C9 | 122.4 (2) |
N1—Co—N2 | 78.14 (8) | C4—C11—C12 | 120.8 (3) |
N1—Co—N3 | 90.62 (8) | C7—C12—C11 | 121.8 (3) |
N2—Co—N3 | 91.58 (8) | N3—C13—C18 | 120.4 (2) |
O1—S—O2 | 111.23 (11) | N3—C13—C14 | 120.1 (2) |
O1—S—O3 | 114.76 (12) | C14—C13—C18 | 119.4 (2) |
O1—S—C16 | 106.28 (12) | C13—C14—C15 | 120.4 (2) |
O2—S—O3 | 111.67 (12) | C14—C15—C16 | 120.1 (2) |
O2—S—C16 | 105.35 (12) | C15—C16—C17 | 119.9 (2) |
O3—S—C16 | 106.85 (11) | S—C16—C15 | 119.86 (18) |
Co—OW1—HW2 | 123.49 | S—C16—C17 | 120.25 (19) |
HW1—OW1—HW2 | 111.84 | C16—C17—C18 | 119.8 (2) |
Co—OW1—HW1 | 124.00 | C13—C18—C17 | 120.5 (2) |
Co—OW2—HW3 | 116.48 | N1—C1—H1 | 118.84 |
HW3—OW2—HW4 | 110.15 | C2—C1—H1 | 118.72 |
Co—OW2—HW4 | 123.89 | C1—C2—H2 | 119.98 |
Co—OW3—HW5 | 115.36 | C3—C2—H2 | 119.96 |
HW5—OW3—HW6 | 117.71 | C2—C3—H3 | 120.13 |
Co—OW3—HW6 | 111.52 | C4—C3—H3 | 120.23 |
Co—N1—C5 | 112.67 (16) | C7—C8—H8 | 120.25 |
C1—N1—C5 | 117.8 (2) | C9—C8—H8 | 120.14 |
Co—N1—C1 | 128.30 (18) | C8—C9—H9 | 119.83 |
C6—N2—C10 | 117.8 (2) | C10—C9—H9 | 119.82 |
Co—N2—C6 | 113.19 (16) | N2—C10—H10 | 118.81 |
Co—N2—C10 | 128.86 (18) | C9—C10—H10 | 118.76 |
Co—N3—C13 | 118.20 (17) | C4—C11—H11 | 119.57 |
Co—N3—H3B | 107.76 | C12—C11—H11 | 119.66 |
C13—N3—H3A | 107.75 | C7—C12—H12 | 119.07 |
C13—N3—H3B | 107.74 | C11—C12—H12 | 119.15 |
H3A—N3—H3B | 107.14 | C13—C14—H14 | 119.80 |
Co—N3—H3A | 107.78 | C15—C14—H14 | 119.77 |
N1—C1—C2 | 122.4 (3) | C14—C15—H15 | 119.90 |
C1—C2—C3 | 120.1 (3) | C16—C15—H15 | 119.98 |
C2—C3—C4 | 119.6 (3) | C16—C17—H17 | 120.17 |
C3—C4—C11 | 124.0 (3) | C18—C17—H17 | 120.08 |
C5—C4—C11 | 119.3 (3) | C13—C18—H18 | 119.80 |
C3—C4—C5 | 116.7 (3) | C17—C18—H18 | 119.73 |
D—H···A | D—H | H···A | D···A | D—H···A |
OW1—HW1···O2i | 0.84 | 1.82 | 2.664 (3) | 177 |
OW1—HW2···Clii | 0.95 | 2.17 | 3.072 (2) | 158 |
OW2—HW3···Cli | 0.97 | 2.06 | 3.018 (2) | 170 |
N3—H3A···O3iii | 0.90 | 2.18 | 3.062 (3) | 167 |
N3—H3B···Clii | 0.90 | 2.53 | 3.392 (2) | 160 |
OW2—HW4···O1i | 0.90 | 2.01 | 2.875 (3) | 161 |
OW3—HW5···O2iii | 0.91 | 1.84 | 2.748 (3) | 174 |
OW3—HW6···O1iv | 0.93 | 1.90 | 2.824 (3) | 170 |
Symmetry codes: (i) x+1/2, −y+1/2, z+1/2; (ii) x−1/2, −y+1/2, z+1/2; (iii) −x−1/2, y−1/2, −z+1/2; (iv) −x+1/2, y−1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Co(C6H6NO3S)(C12H8N2)(H2O)3]Cl |
Mr | 500.81 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 7.0148 (10), 15.896 (4), 18.587 (5) |
β (°) | 96.548 (18) |
V (Å3) | 2059.0 (8) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.11 |
Crystal size (mm) | 0.50 × 0.38 × 0.32 |
Data collection | |
Diffractometer | Siemens P4 diffractometer |
Absorption correction | ψ scan (SHELXTL; Siemens, 1994) |
Tmin, Tmax | 0.561, 0.687 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5562, 4060, 2959 |
Rint | 0.026 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.073, 1.09 |
No. of reflections | 4060 |
No. of parameters | 271 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.31, −0.37 |
Computer programs: XSCANS (Siemens, 1994), XSCANS, SHELXTL (Siemens, 1994), SHELXTL.
Co—OW1 | 2.065 (2) | S—O3 | 1.4415 (18) |
Co—OW2 | 2.083 (2) | S—C16 | 1.767 (2) |
Co—OW3 | 2.091 (2) | N1—C1 | 1.329 (3) |
Co—N1 | 2.119 (2) | N1—C5 | 1.361 (3) |
Co—N2 | 2.116 (2) | N2—C10 | 1.333 (3) |
Co—N3 | 2.270 (2) | N2—C6 | 1.360 (3) |
S—O1 | 1.461 (2) | N3—C13 | 1.428 (3) |
S—O2 | 1.469 (2) | ||
OW1—Co—OW2 | 90.81 (8) | O2—S—C16 | 105.35 (12) |
OW1—Co—OW3 | 92.55 (8) | O3—S—C16 | 106.85 (11) |
OW1—Co—N1 | 170.16 (8) | Co—N1—C5 | 112.67 (16) |
OW1—Co—N2 | 94.96 (8) | C1—N1—C5 | 117.8 (2) |
OW1—Co—N3 | 82.49 (8) | Co—N1—C1 | 128.30 (18) |
OW2—Co—OW3 | 86.49 (8) | C6—N2—C10 | 117.8 (2) |
OW2—Co—N1 | 96.43 (8) | Co—N2—C6 | 113.19 (16) |
OW2—Co—N2 | 92.36 (8) | Co—N2—C10 | 128.86 (18) |
OW2—Co—N3 | 172.50 (8) | Co—N3—C13 | 118.20 (17) |
OW3—Co—N1 | 94.52 (8) | N1—C1—C2 | 122.4 (3) |
OW3—Co—N2 | 172.41 (8) | N1—C5—C6 | 117.1 (2) |
OW3—Co—N3 | 90.43 (8) | N1—C5—C4 | 123.3 (2) |
N1—Co—N2 | 78.14 (8) | N2—C6—C5 | 117.1 (2) |
N1—Co—N3 | 90.62 (8) | N2—C6—C7 | 122.8 (2) |
N2—Co—N3 | 91.58 (8) | N2—C10—C9 | 122.4 (2) |
O1—S—O2 | 111.23 (11) | N3—C13—C18 | 120.4 (2) |
O1—S—O3 | 114.76 (12) | N3—C13—C14 | 120.1 (2) |
O1—S—C16 | 106.28 (12) | S—C16—C15 | 119.86 (18) |
O2—S—O3 | 111.67 (12) | S—C16—C17 | 120.25 (19) |
D—H···A | D—H | H···A | D···A | D—H···A |
OW1—HW1···O2i | 0.84 | 1.82 | 2.664 (3) | 177 |
OW1—HW2···Clii | 0.95 | 2.17 | 3.072 (2) | 158 |
OW2—HW3···Cli | 0.97 | 2.06 | 3.018 (2) | 170 |
N3—H3A···O3iii | 0.90 | 2.18 | 3.062 (3) | 167 |
N3—H3B···Clii | 0.90 | 2.53 | 3.392 (2) | 160 |
OW2—HW4···O1i | 0.90 | 2.01 | 2.875 (3) | 161 |
OW3—HW5···O2iii | 0.91 | 1.84 | 2.748 (3) | 174 |
OW3—HW6···O1iv | 0.93 | 1.90 | 2.824 (3) | 170 |
Symmetry codes: (i) x+1/2, −y+1/2, z+1/2; (ii) x−1/2, −y+1/2, z+1/2; (iii) −x−1/2, y−1/2, −z+1/2; (iv) −x+1/2, y−1/2, −z+1/2. |
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Supramolecular frameworks based on metal and organic building blocks that contain diverse topologies with desired features are increasing receiving attention, because of their promising potential properties in catalysis (Fujita et al., 1994), gas storage (Kitaura et al., 2003) and magnetism (Inoue et al., 1996). However, there have been few reports of metal-based organosulfonate anions containing supramolecular compounds to date (Cai et al., 2001a; Cai et al., 2001b; Wang et al., 2002). We present here a novel compound, [Co(H2O)3(C6H6NO3S)(C12H8N2)]+Cl− (1), built from discrete [Co(H2O)3(C6H6NO3S)(C12H8N2)]+ cations, each formed by one 4-aminobenzenesulfonate (4-ABS) ligand, one 1,10-phenanthroline (1,10-phen) ligand and three coordinated water molecules, and one uncoordinated chlorine anion.
As depicted by Fig. 1, the CoII center exhibits slightly distorted octahedral coordination geometry, defined by three aqua O atoms [Co—OW1 = 2.065 (2) Å, Co—OW2 = 2.083 (2) Å and Co—OW3 = 2.0912 (18) Å], and two N atoms from a 1,10-phen ligand [Co—N1 = 2.119 (2) Å and Co—N2 = 2.116 (2) Å], and an N atom donor from a 4-ABS ligand [Co—N3 = 2.270 (2) Å]. The coordination environment and mode of 4-ABS differ from that in [Co(H2O)4(4-ABS)2(4,4'-bipy)]·H2O (Wang et al., 2002), in which the 4-ABS ligands are not coordinated to CoII and form one-dimensional head-to-tail zigzag chains via hydrogen-bonding interactions. The two different rings from the 4-ABS and 1,10-phen groups are not completely parallel to one another, the dihedral angles between their planes being 12.6° and their average ring separation being 3.324 Å.
As shown in Fig. 2, these discrete [Co(H2O)3(C6H6NO3S)(C12H8N2)]+ cations and chloride anions are connected into a two-dimensional supramolecular motif. The rings of two 4-ABS and two 1,10-phen ligands from two different discrete cations lie parallel to one another. In the supramolecular architecture, unusual hydrogen-bonding interactions play a crucial role. The coordinated water molecules (OW2 and OW1) from one [Co(H2O)3(4-ABS)(1,10-phen)]+ cation interact with the SO3− group of the 4-ABS ligand from another, thus forming hydrogen-bonding interactions. ##AUTHOR: Supply s.u.'s for all the following O···O and Cl···O distances: [OW2A···O1 = 2.875 (2) and OW2A···O1(2) = 2.664(?) Å]. Furthermore, the coordinated water molecules (OW2 and OW1) from two adjacent cations are bridged via hydrogen-bonding interactions with a chloride anion [Cl···OW1 = 3.072(?) Å and Cl···OW2 = 3.018(?) Å]. In addition, there are hydrogen-bonding interactions between the OW3 coordinated water molecules and the SO3− groups of 4-ABS anions from two adjacent building blocks [O1···OW3 = 2.824(?)Å and O2···OW3 = 2.748(?) Å]. Therefore, such hydrogen-bonding interactions consolidate the structural architecture and further extend the two-dimensional supramolecular structure into a three-dimensional network containing many nanocavities formed by hydrogen bonds (see Fig. 3). ##AUTHOR: Are these "nanocavities" still present when (a) H atoms are considered and (b) van der Waals radii are used? Please check. If they are present I would expect to find voids in the structure.