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The reaction of 2-(2-pyridylmethylamino)ethanesulfonic acid (HPMT) with CoCl2·6H2O in water gave the mononuclear title complex, [Co(PMT)2] or [Co(C8H11N2O3S)2]. The CoII atom lies on a centre of symmetry and the two deprotonated HPMT anions coordinate to Co in a facial arrangement as N,N′,O-tridentate donor ligands.
Supporting information
CCDC reference: 614216
Key indicators
- Single-crystal X-ray study
- T = 291 K
- Mean (C-C) = 0.003 Å
- R factor = 0.023
- wR factor = 0.061
- Data-to-parameter ratio = 17.1
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.54 Ratio
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - N1 .. 5.36 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - N2 .. 7.10 su
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 4
O2 -CO1 -O2 -S1 4.00 0.00 3.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 13
N1 -CO1 -N1 -C5 57.00 4.00 3.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 18
N1 -CO1 -N1 -C1 -129.00 4.00 3.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 21
N2 -CO1 -N2 -C6 -69.00 9.00 3.555 1.555 1.555 1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 26
N2 -CO1 -N2 -C7 168.00 9.00 3.555 1.555 1.555 1.555
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
10 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
3 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
6 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2; data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2004); software used to prepare material for publication: SHELXTL.
Bis[2-(2-pyridylmethylamino)ethanesulfonato-
κ3N,
N',
O]cobalt(II)
top
Crystal data top
[Co(C8H11N2O3S)2] | F(000) = 506 |
Mr = 489.43 | Dx = 1.545 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 4005 reflections |
a = 9.6066 (12) Å | θ = 2.8–28.2° |
b = 9.9919 (12) Å | µ = 1.05 mm−1 |
c = 11.4099 (14) Å | T = 291 K |
β = 106.127 (1)° | Block, red |
V = 1052.1 (2) Å3 | 0.51 × 0.33 × 0.30 mm |
Z = 2 | |
Data collection top
Bruker APEX-II CCD area-detector diffractometer | 2348 independent reflections |
Radiation source: fine-focus sealed tube | 2149 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.012 |
φ and ω scans | θmax = 27.5°, θmin = 2.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −10→12 |
Tmin = 0.615, Tmax = 0.743 | k = −12→12 |
6149 measured reflections | l = −14→14 |
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)] = 0.023 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.061 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0276P)2 + 0.4686P] where P = (Fo2 + 2Fc2)/3 |
2348 reflections | (Δ/σ)max < 0.001 |
137 parameters | Δρmax = 0.23 e Å−3 |
0 restraints | Δρmin = −0.27 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 | 0.02237 (8) | |
S1 | −0.13176 (4) | 0.29148 (3) | 0.04222 (3) | 0.02834 (10) | |
O1 | −0.05128 (15) | 0.39683 (11) | 0.11997 (10) | 0.0452 (3) | |
O2 | −0.07244 (13) | 0.15923 (10) | 0.08798 (10) | 0.0364 (3) | |
O3 | −0.28625 (14) | 0.29965 (16) | 0.02250 (14) | 0.0580 (4) | |
N1 | 0.22226 (14) | 0.03663 (13) | 0.10627 (12) | 0.0303 (3) | |
N2 | 0.07757 (14) | 0.13428 (12) | −0.11636 (11) | 0.0275 (3) | |
C1 | 0.28036 (19) | 0.02079 (17) | 0.22774 (16) | 0.0397 (4) | |
H1 | 0.2248 | −0.0193 | 0.2729 | 0.048* | |
C2 | 0.4187 (2) | 0.0618 (3) | 0.2869 (2) | 0.0621 (6) | |
H2 | 0.4558 | 0.0498 | 0.3706 | 0.075* | |
C3 | 0.5012 (2) | 0.1209 (3) | 0.2202 (2) | 0.0745 (7) | |
H3 | 0.5946 | 0.1502 | 0.2586 | 0.089* | |
C4 | 0.4442 (2) | 0.1366 (2) | 0.0954 (2) | 0.0589 (5) | |
H4 | 0.4989 | 0.1758 | 0.0489 | 0.071* | |
C5 | 0.30410 (16) | 0.09274 (16) | 0.04109 (15) | 0.0350 (3) | |
C6 | 0.23367 (17) | 0.10317 (17) | −0.09403 (16) | 0.0371 (4) | |
H6A | 0.2803 | 0.1731 | −0.1284 | 0.045* | |
H6B | 0.2448 | 0.0193 | −0.1333 | 0.045* | |
C7 | 0.05744 (17) | 0.28002 (14) | −0.10000 (14) | 0.0310 (3) | |
H7A | 0.0829 | 0.3290 | −0.1645 | 0.037* | |
H7B | 0.1221 | 0.3086 | −0.0227 | 0.037* | |
C8 | −0.09754 (17) | 0.31302 (15) | −0.10236 (13) | 0.0293 (3) | |
H8A | −0.1628 | 0.2560 | −0.1617 | 0.035* | |
H8B | −0.1180 | 0.4051 | −0.1285 | 0.035* | |
H2A | 0.036 (2) | 0.1156 (18) | −0.1906 (17) | 0.038 (5)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.02290 (14) | 0.02102 (13) | 0.02362 (14) | −0.00264 (10) | 0.00716 (10) | 0.00039 (9) |
S1 | 0.0330 (2) | 0.02566 (18) | 0.02802 (18) | 0.00023 (14) | 0.01128 (14) | −0.00099 (13) |
O1 | 0.0735 (9) | 0.0313 (6) | 0.0323 (6) | −0.0113 (6) | 0.0172 (6) | −0.0075 (5) |
O2 | 0.0580 (7) | 0.0264 (5) | 0.0296 (5) | 0.0042 (5) | 0.0200 (5) | 0.0022 (4) |
O3 | 0.0351 (7) | 0.0812 (11) | 0.0629 (9) | 0.0088 (7) | 0.0220 (6) | 0.0115 (8) |
N1 | 0.0261 (6) | 0.0303 (6) | 0.0333 (6) | −0.0017 (5) | 0.0064 (5) | −0.0012 (5) |
N2 | 0.0308 (7) | 0.0274 (6) | 0.0259 (6) | −0.0019 (5) | 0.0104 (5) | 0.0000 (5) |
C1 | 0.0374 (9) | 0.0430 (9) | 0.0347 (8) | 0.0027 (7) | 0.0035 (7) | −0.0027 (7) |
C2 | 0.0432 (11) | 0.0823 (15) | 0.0476 (11) | 0.0035 (11) | −0.0094 (9) | −0.0075 (11) |
C3 | 0.0296 (10) | 0.101 (2) | 0.0796 (16) | −0.0131 (11) | −0.0067 (10) | −0.0137 (14) |
C4 | 0.0287 (9) | 0.0691 (14) | 0.0793 (15) | −0.0117 (9) | 0.0159 (9) | −0.0003 (11) |
C5 | 0.0246 (7) | 0.0345 (8) | 0.0475 (9) | −0.0008 (6) | 0.0128 (6) | −0.0003 (7) |
C6 | 0.0349 (8) | 0.0392 (8) | 0.0447 (9) | −0.0021 (7) | 0.0233 (7) | 0.0043 (7) |
C7 | 0.0376 (8) | 0.0255 (7) | 0.0322 (7) | −0.0045 (6) | 0.0135 (6) | 0.0027 (6) |
C8 | 0.0355 (8) | 0.0269 (7) | 0.0242 (7) | 0.0013 (6) | 0.0062 (6) | 0.0031 (5) |
Geometric parameters (Å, º) top
Co1—O2 | 2.1004 (11) | C1—H1 | 0.9300 |
Co1—O2i | 2.1004 (11) | C2—C3 | 1.375 (4) |
Co1—N2i | 2.1604 (12) | C2—H2 | 0.9300 |
Co1—N2 | 2.1605 (12) | C3—C4 | 1.385 (3) |
Co1—N1i | 2.1737 (13) | C3—H3 | 0.9300 |
Co1—N1 | 2.1737 (13) | C4—C5 | 1.387 (2) |
S1—O3 | 1.4403 (14) | C4—H4 | 0.9300 |
S1—O1 | 1.4532 (12) | C5—C6 | 1.505 (2) |
S1—O2 | 1.4758 (11) | C6—H6A | 0.9700 |
S1—C8 | 1.7824 (15) | C6—H6B | 0.9700 |
N1—C5 | 1.345 (2) | C7—C8 | 1.518 (2) |
N1—C1 | 1.352 (2) | C7—H7A | 0.9700 |
N2—C6 | 1.483 (2) | C7—H7B | 0.9700 |
N2—C7 | 1.4876 (19) | C8—H8A | 0.9700 |
N2—H2A | 0.851 (19) | C8—H8B | 0.9700 |
C1—C2 | 1.375 (3) | | |
| | | |
O2—Co1—O2i | 180.0 | N1—C1—H1 | 118.8 |
O2—Co1—N2i | 87.71 (5) | C2—C1—H1 | 118.8 |
O2i—Co1—N2i | 92.29 (5) | C1—C2—C3 | 118.9 (2) |
O2—Co1—N2 | 92.29 (5) | C1—C2—H2 | 120.5 |
O2i—Co1—N2 | 87.71 (5) | C3—C2—H2 | 120.5 |
N2i—Co1—N2 | 180.0 | C2—C3—C4 | 119.59 (19) |
O2—Co1—N1i | 89.41 (5) | C2—C3—H3 | 120.2 |
O2i—Co1—N1i | 90.59 (5) | C4—C3—H3 | 120.2 |
N2i—Co1—N1i | 77.60 (5) | C3—C4—C5 | 118.7 (2) |
N2—Co1—N1i | 102.40 (5) | C3—C4—H4 | 120.6 |
O2—Co1—N1 | 90.60 (5) | C5—C4—H4 | 120.6 |
O2i—Co1—N1 | 89.41 (5) | N1—C5—C4 | 121.89 (17) |
N2i—Co1—N1 | 102.40 (5) | N1—C5—C6 | 115.44 (13) |
N2—Co1—N1 | 77.60 (5) | C4—C5—C6 | 122.67 (16) |
N1i—Co1—N1 | 180.0 | N2—C6—C5 | 109.63 (12) |
O3—S1—O1 | 113.87 (9) | N2—C6—H6A | 109.7 |
O3—S1—O2 | 112.70 (8) | C5—C6—H6A | 109.7 |
O1—S1—O2 | 110.18 (7) | N2—C6—H6B | 109.7 |
O3—S1—C8 | 107.19 (8) | C5—C6—H6B | 109.7 |
O1—S1—C8 | 105.89 (7) | H6A—C6—H6B | 108.2 |
O2—S1—C8 | 106.45 (7) | N2—C7—C8 | 111.81 (12) |
S1—O2—Co1 | 130.98 (6) | N2—C7—H7A | 109.3 |
C5—N1—C1 | 118.50 (14) | C8—C7—H7A | 109.3 |
C5—N1—Co1 | 113.33 (10) | N2—C7—H7B | 109.3 |
C1—N1—Co1 | 127.88 (12) | C8—C7—H7B | 109.3 |
C6—N2—C7 | 110.14 (12) | H7A—C7—H7B | 107.9 |
C6—N2—Co1 | 105.62 (9) | C7—C8—S1 | 112.92 (10) |
C7—N2—Co1 | 116.86 (9) | C7—C8—H8A | 109.0 |
C6—N2—H2A | 107.5 (13) | S1—C8—H8A | 109.0 |
C7—N2—H2A | 107.3 (12) | C7—C8—H8B | 109.0 |
Co1—N2—H2A | 109.1 (12) | S1—C8—H8B | 109.0 |
N1—C1—C2 | 122.39 (19) | H8A—C8—H8B | 107.8 |
| | | |
O3—S1—O2—Co1 | 104.90 (11) | N2i—Co1—N2—C7 | 168 (9) |
O1—S1—O2—Co1 | −126.71 (10) | N1i—Co1—N2—C7 | 89.74 (11) |
C8—S1—O2—Co1 | −12.33 (12) | N1—Co1—N2—C7 | −90.27 (11) |
O2i—Co1—O2—S1 | −43 (100) | C5—N1—C1—C2 | 1.1 (3) |
N2i—Co1—O2—S1 | −147.24 (10) | Co1—N1—C1—C2 | −172.37 (15) |
N2—Co1—O2—S1 | 32.76 (10) | N1—C1—C2—C3 | −0.1 (3) |
N1i—Co1—O2—S1 | −69.63 (10) | C1—C2—C3—C4 | −0.7 (4) |
N1—Co1—O2—S1 | 110.36 (10) | C2—C3—C4—C5 | 0.5 (4) |
O2—Co1—N1—C5 | −106.87 (11) | C1—N1—C5—C4 | −1.2 (2) |
O2i—Co1—N1—C5 | 73.13 (11) | Co1—N1—C5—C4 | 173.11 (15) |
N2i—Co1—N1—C5 | 165.34 (11) | C1—N1—C5—C6 | 178.19 (14) |
N2—Co1—N1—C5 | −14.66 (11) | Co1—N1—C5—C6 | −7.46 (17) |
N1i—Co1—N1—C5 | 57 (4) | C3—C4—C5—N1 | 0.5 (3) |
O2—Co1—N1—C1 | 66.84 (14) | C3—C4—C5—C6 | −178.9 (2) |
O2i—Co1—N1—C1 | −113.16 (14) | C7—N2—C6—C5 | 80.94 (15) |
N2i—Co1—N1—C1 | −20.95 (14) | Co1—N2—C6—C5 | −46.08 (14) |
N2—Co1—N1—C1 | 159.05 (14) | N1—C5—C6—N2 | 36.88 (19) |
N1i—Co1—N1—C1 | −129 (4) | C4—C5—C6—N2 | −143.69 (17) |
O2—Co1—N2—C6 | 122.68 (10) | C6—N2—C7—C8 | −171.04 (12) |
O2i—Co1—N2—C6 | −57.32 (10) | Co1—N2—C7—C8 | −50.57 (14) |
N2i—Co1—N2—C6 | −69 (9) | N2—C7—C8—S1 | 84.43 (13) |
N1i—Co1—N2—C6 | −147.43 (10) | O3—S1—C8—C7 | −168.79 (11) |
N1—Co1—N2—C6 | 32.57 (10) | O1—S1—C8—C7 | 69.31 (12) |
O2—Co1—N2—C7 | −0.16 (11) | O2—S1—C8—C7 | −47.96 (12) |
O2i—Co1—N2—C7 | 179.84 (11) | | |
Symmetry code: (i) −x, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2A···O1ii | 0.851 (19) | 2.094 (19) | 2.9345 (17) | 169.4 (17) |
Symmetry code: (ii) x, −y+1/2, z−1/2. |
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