The structure of the title complex consists of neutral molecules of [Co(nbs)2(H2O)4] (nbs is the p-nitrobenzoxasulfamate anion, C6H3N2O5S−). The Co2+ ion occupies an inversion centre and exhibits a distorted octahedral geometry, involving two monodentate nbs (Nimine) anions and four water molecules. The crystal structure is stabilized by hydrogen bonding and weak aromatic π–π stacking interactions between the benzene rings of nbs ligands, forming a three-dimensional network.
Supporting information
CCDC reference: 238667
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.004 Å
- R factor = 0.037
- wR factor = 0.100
- Data-to-parameter ratio = 9.9
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 9.86
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
0 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: X-AREA (Stoe & Cie, 2002); cell refinement: X-AREA; data reduction: X-RED (Stoe & Cie, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).
trans-Tetraaquabis(
p-nitrobenzoxasulfamato)cobalt(II)
top
Crystal data top
[Co(C6H3N2O5S)2(H2O)4] | Z = 1 |
Mr = 561.32 | F(000) = 285 |
Triclinic, P1 | Dx = 1.972 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.2079 (9) Å | Cell parameters from 11439 reflections |
b = 7.3251 (10) Å | θ = 2.0–25.2° |
c = 10.4032 (14) Å | µ = 1.22 mm−1 |
α = 88.760 (11)° | T = 293 K |
β = 77.191 (10)° | Prismatic, brown |
γ = 62.442 (9)° | 0.5 × 0.4 × 0.1 mm |
V = 472.75 (11) Å3 | |
Data collection top
Stoe IPDS-II diffractometer | 1647 independent reflections |
Radiation source: fine-focus sealed tube | 1571 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.064 |
Detector resolution: 6.67 pixels mm-1 | θmax = 25.0°, θmin = 2.0° |
rotation method scans | h = −8→8 |
Absorption correction: integration (X-RED; Stoe & Cie, 2002) | k = −8→8 |
Tmin = 0.563, Tmax = 0.885 | l = −12→12 |
5264 measured reflections | |
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)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.100 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0729P)2 + 0.0979P] where P = (Fo2 + 2Fc2)/3 |
1647 reflections | (Δ/σ)max = 0.001 |
167 parameters | Δρmax = 0.93 e Å−3 |
4 restraints | Δρmin = −0.67 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Co1 | 0.0000 | 0.0000 | 0.0000 | 0.02352 (19) | |
S1 | 0.20322 (9) | 0.18184 (8) | 0.18616 (5) | 0.0274 (2) | |
N1 | 0.0182 (3) | 0.1215 (3) | 0.18206 (16) | 0.0280 (4) | |
N2 | −0.4760 (3) | 0.3635 (3) | 0.69980 (18) | 0.0357 (5) | |
O1W | 0.3165 (3) | −0.2299 (3) | −0.02973 (16) | 0.0369 (4) | |
O2W | 0.0879 (3) | 0.2032 (3) | −0.10933 (16) | 0.0391 (4) | |
O1 | 0.1910 (3) | 0.3544 (3) | 0.11558 (19) | 0.0452 (4) | |
O2 | 0.4131 (3) | 0.0073 (3) | 0.15810 (18) | 0.0411 (4) | |
O3 | 0.1385 (3) | 0.2544 (3) | 0.34345 (16) | 0.0403 (4) | |
O4 | −0.6546 (3) | 0.3721 (3) | 0.72894 (16) | 0.0463 (5) | |
O5 | −0.4080 (4) | 0.4261 (3) | 0.77740 (17) | 0.0502 (5) | |
C1 | −0.1129 (4) | 0.1621 (3) | 0.30800 (19) | 0.0260 (4) | |
C2 | −0.0459 (4) | 0.2394 (3) | 0.4011 (2) | 0.0292 (5) | |
C3 | −0.1545 (4) | 0.3006 (3) | 0.5306 (2) | 0.0319 (5) | |
H3 | −0.1061 | 0.3514 | 0.5898 | 0.038* | |
C4 | −0.3414 (4) | 0.2821 (3) | 0.5679 (2) | 0.0303 (5) | |
C5 | −0.4132 (4) | 0.2036 (3) | 0.4808 (2) | 0.0318 (5) | |
H5 | −0.5392 | 0.1930 | 0.5101 | 0.038* | |
C6 | −0.2979 (4) | 0.1409 (4) | 0.3505 (2) | 0.0304 (5) | |
H6 | −0.3437 | 0.0854 | 0.2923 | 0.037* | |
H1A | 0.393 (6) | −0.342 (4) | −0.085 (3) | 0.067 (10)* | |
H1B | 0.418 (6) | −0.255 (7) | 0.012 (4) | 0.098 (15)* | |
H2A | 0.218 (3) | 0.184 (6) | −0.126 (3) | 0.066 (11)* | |
H2B | −0.011 (5) | 0.325 (4) | −0.114 (4) | 0.081 (13)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.0223 (3) | 0.0253 (3) | 0.0259 (3) | −0.0138 (2) | −0.00520 (17) | 0.00219 (16) |
S1 | 0.0261 (4) | 0.0308 (3) | 0.0319 (3) | −0.0185 (3) | −0.0076 (2) | 0.0030 (2) |
N1 | 0.0275 (10) | 0.0331 (9) | 0.0296 (9) | −0.0197 (8) | −0.0054 (7) | 0.0005 (7) |
N2 | 0.0399 (13) | 0.0266 (9) | 0.0312 (9) | −0.0106 (9) | −0.0027 (8) | 0.0046 (7) |
O1W | 0.0271 (9) | 0.0391 (9) | 0.0399 (9) | −0.0108 (8) | −0.0093 (7) | −0.0050 (7) |
O2W | 0.0444 (11) | 0.0380 (9) | 0.0411 (9) | −0.0269 (9) | −0.0044 (7) | 0.0058 (7) |
O1 | 0.0504 (12) | 0.0426 (9) | 0.0596 (11) | −0.0331 (9) | −0.0205 (9) | 0.0174 (8) |
O2 | 0.0267 (10) | 0.0418 (10) | 0.0536 (10) | −0.0153 (8) | −0.0084 (8) | 0.0003 (7) |
O3 | 0.0382 (10) | 0.0605 (11) | 0.0342 (8) | −0.0347 (9) | −0.0037 (7) | −0.0065 (7) |
O4 | 0.0386 (11) | 0.0457 (10) | 0.0425 (9) | −0.0158 (8) | 0.0033 (8) | 0.0072 (7) |
O5 | 0.0569 (13) | 0.0545 (11) | 0.0329 (9) | −0.0230 (10) | −0.0053 (8) | −0.0078 (8) |
C1 | 0.0285 (12) | 0.0226 (9) | 0.0281 (9) | −0.0128 (9) | −0.0072 (8) | 0.0034 (7) |
C2 | 0.0285 (12) | 0.0297 (10) | 0.0334 (10) | −0.0166 (9) | −0.0086 (8) | 0.0041 (8) |
C3 | 0.0365 (13) | 0.0325 (11) | 0.0298 (10) | −0.0178 (10) | −0.0099 (9) | −0.0001 (8) |
C4 | 0.0337 (12) | 0.0243 (10) | 0.0292 (10) | −0.0118 (9) | −0.0047 (8) | 0.0041 (8) |
C5 | 0.0304 (12) | 0.0297 (10) | 0.0372 (11) | −0.0172 (9) | −0.0048 (9) | 0.0058 (8) |
C6 | 0.0290 (13) | 0.0328 (11) | 0.0346 (11) | −0.0185 (10) | −0.0079 (9) | 0.0011 (8) |
Geometric parameters (Å, º) top
Co1—O1W | 2.0713 (18) | O1W—H1A | 0.876 (18) |
Co1—O1Wi | 2.0713 (18) | O1W—H1B | 0.88 (5) |
Co1—O2W | 2.0951 (16) | O2W—H2A | 0.860 (19) |
Co1—O2Wi | 2.0951 (16) | O2W—H2B | 0.857 (19) |
Co1—N1i | 2.1653 (16) | O3—C2 | 1.385 (3) |
Co1—N1 | 2.1653 (16) | C1—C6 | 1.388 (3) |
S1—O1 | 1.4251 (18) | C1—C2 | 1.405 (3) |
S1—O2 | 1.428 (2) | C2—C3 | 1.364 (3) |
S1—N1 | 1.5958 (18) | C3—C4 | 1.385 (3) |
S1—O3 | 1.6270 (16) | C3—H3 | 0.9300 |
N1—C1 | 1.381 (3) | C4—C5 | 1.388 (3) |
N2—O5 | 1.225 (3) | C5—C6 | 1.383 (3) |
N2—O4 | 1.227 (3) | C5—H5 | 0.9300 |
N2—C4 | 1.445 (3) | C6—H6 | 0.9300 |
| | | |
O1W—Co1—O1Wi | 180.00 (17) | O4—N2—C4 | 119.3 (2) |
O1W—Co1—O2W | 92.89 (8) | Co1—O1W—H1A | 132 (3) |
O1Wi—Co1—O2W | 87.11 (8) | Co1—O1W—H1B | 133 (3) |
O1W—Co1—O2Wi | 87.11 (8) | H1A—O1W—H1B | 95 (4) |
O1Wi—Co1—O2Wi | 92.89 (8) | Co1—O2W—H2A | 121 (3) |
O2W—Co1—O2Wi | 180.00 (13) | Co1—O2W—H2B | 118 (3) |
O1W—Co1—N1i | 89.05 (7) | H2A—O2W—H2B | 118 (4) |
O1Wi—Co1—N1i | 90.95 (7) | C2—O3—S1 | 108.07 (13) |
O2W—Co1—N1i | 88.45 (7) | N1—C1—C6 | 128.66 (19) |
O2Wi—Co1—N1i | 91.55 (7) | N1—C1—C2 | 113.05 (19) |
O1W—Co1—N1 | 90.95 (7) | C6—C1—C2 | 118.27 (19) |
O1Wi—Co1—N1 | 89.05 (7) | C3—C2—O3 | 124.28 (19) |
O2W—Co1—N1 | 91.55 (7) | C3—C2—C1 | 124.2 (2) |
O2Wi—Co1—N1 | 88.45 (7) | O3—C2—C1 | 111.46 (18) |
N1i—Co1—N1 | 180.00 (4) | C2—C3—C4 | 115.60 (19) |
O1—S1—O2 | 113.98 (12) | C2—C3—H3 | 122.2 |
O1—S1—N1 | 114.63 (11) | C4—C3—H3 | 122.2 |
O2—S1—N1 | 112.83 (10) | C3—C4—C5 | 122.7 (2) |
O1—S1—O3 | 107.65 (11) | C3—C4—N2 | 118.6 (2) |
O2—S1—O3 | 107.14 (11) | C5—C4—N2 | 118.6 (2) |
N1—S1—O3 | 99.09 (9) | C6—C5—C4 | 120.2 (2) |
C1—N1—S1 | 108.29 (14) | C6—C5—H5 | 119.9 |
C1—N1—Co1 | 130.21 (15) | C4—C5—H5 | 119.9 |
S1—N1—Co1 | 121.50 (10) | C5—C6—C1 | 119.0 (2) |
O5—N2—O4 | 122.6 (2) | C5—C6—H6 | 120.5 |
O5—N2—C4 | 118.1 (2) | C1—C6—H6 | 120.5 |
| | | |
O1—S1—N1—C1 | −112.54 (16) | Co1—N1—C1—C2 | 179.45 (14) |
O2—S1—N1—C1 | 114.77 (16) | S1—O3—C2—C3 | −175.52 (19) |
O3—S1—N1—C1 | 1.74 (16) | S1—O3—C2—C1 | 1.7 (2) |
O1—S1—N1—Co1 | 67.14 (15) | N1—C1—C2—C3 | 176.7 (2) |
O2—S1—N1—Co1 | −65.55 (14) | C6—C1—C2—C3 | −1.9 (3) |
O3—S1—N1—Co1 | −178.58 (11) | N1—C1—C2—O3 | −0.6 (3) |
O1W—Co1—N1—C1 | −126.65 (19) | C6—C1—C2—O3 | −179.12 (19) |
O1Wi—Co1—N1—C1 | 53.35 (19) | O3—C2—C3—C4 | 177.0 (2) |
O2W—Co1—N1—C1 | 140.43 (19) | C1—C2—C3—C4 | 0.1 (3) |
O2Wi—Co1—N1—C1 | −39.57 (19) | C2—C3—C4—C5 | 1.0 (3) |
O1W—Co1—N1—S1 | 53.74 (12) | C2—C3—C4—N2 | −173.76 (18) |
O1Wi—Co1—N1—S1 | −126.25 (12) | O5—N2—C4—C3 | −7.4 (3) |
O2W—Co1—N1—S1 | −39.17 (12) | O4—N2—C4—C3 | 170.9 (2) |
O2Wi—Co1—N1—S1 | 140.83 (12) | O5—N2—C4—C5 | 177.6 (2) |
O1—S1—O3—C2 | 117.53 (17) | O4—N2—C4—C5 | −4.1 (3) |
O2—S1—O3—C2 | −119.48 (16) | C3—C4—C5—C6 | −0.4 (3) |
N1—S1—O3—C2 | −2.07 (17) | N2—C4—C5—C6 | 174.40 (19) |
S1—N1—C1—C6 | 177.46 (19) | C4—C5—C6—C1 | −1.4 (3) |
Co1—N1—C1—C6 | −2.2 (3) | N1—C1—C6—C5 | −175.9 (2) |
S1—N1—C1—C2 | −0.9 (2) | C2—C1—C6—C5 | 2.4 (3) |
Symmetry code: (i) −x, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1A···O5ii | 0.88 (3) | 1.99 (3) | 2.853 (2) | 171 (4) |
O1W—H1B···O2 | 0.88 (5) | 2.46 (4) | 3.031 (2) | 123 (3) |
O1W—H1B···O1iii | 0.88 (5) | 2.59 (5) | 3.141 (3) | 121 (3) |
O1W—H1B···O5iv | 0.88 (5) | 2.50 (4) | 3.020 (3) | 118 (4) |
O2W—H2A···O4v | 0.86 (3) | 2.34 (3) | 2.908 (2) | 124 (3) |
O2W—H2A···O2iii | 0.86 (3) | 2.31 (3) | 3.109 (3) | 156 (3) |
O2W—H2B···O1vi | 0.86 (3) | 2.09 (3) | 2.927 (3) | 164 (4) |
Symmetry codes: (ii) x+1, y−1, z−1; (iii) −x+1, −y, −z; (iv) −x, −y, −z+1; (v) x+1, y, z−1; (vi) −x, −y+1, −z. |