Literature DB >> 21578676

Tetra-aqua-bis(pyridine-κN)cobalt(II) bis-[4-amino-N-(6-chloro-pyridazin-3-yl)benzene-sulfonamidate].

Nan Li1, Hong-Li Zou, Xiao-Yan Song, Yan-Cheng Liu, Zhen-Feng Chen.   

Abstract

The structure of the title compound, [Co(C(5)H(5)N)(2)(H(2)O)(4)](C(10)H(8)ClN(4)O(2)S)(2), consists of a discrete tetra-aqua-bis(pyridine-κN)cobalt(II) cation and two 4-amino-N-(6-chloro-pyridazin-3-yl)benzene-sulfonamidate anions. In the cation, the Co(II) ion sits on an inversion centre and is octa-hedrally coordinated by two pyridine N atoms and four O atoms. A two-dimensional network parallel to (010) is formed via inter-molecular O-H⋯O, O-H⋯N, N-H⋯N and N-H⋯O hydrogen bonds.

Entities:  

Year:  2009        PMID： 21578676      PMCID： PMC2971792          DOI： 10.1107/S1600536809049599

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For the structure of sulfachloro­pyridazine, see: Tan et al. (2005 ▶). For a sulfachloro­pyridazine–metal complex, see: Fogg et al. (1995 ▶). For an aqua­n class="Chemical">pyridine–cobalt(II) complex, see: Clegg et al. (2006 ▶).

Experimental

Crystal data

[Co(C5H5N)2(H2O)4](C10H8ClN4O2S)2 M = 856.62 Monoclinic, a = 8.5897 (12) Å b = 25.807 (3) Å c = 8.5338 (12) Å β = 101.694 (3)° V = 1852.5 (4) Å3 Z = 2 Mo Kα radiation μ = 0.78 mm−1 T = 193 K 0.21 × 0.15 × 0.12 mm

Data collection

Rigaku Mercury CCD diffractometer Absorption correction: multi-scan (REQAB; Jacobson, 1998 ▶) T min = 0.853, T max = 0.912 20359 measured reflections 4226 independent reflections 3331 reflections with I > 2σ(I) R int = 0.050

Refinement

R[F 2 > 2σ(F 2)] = 0.054 wR(F 2) = 0.108 S = 1.14 4226 reflections 258 parameters 1 restraint H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.66 e Å−3 Δρmin = −0.45 e Å−3 Data collection: CrystalClear (Rigaku, 1999 ▶); cell refinement: CrystalClear; data reduction: CrystalStructure (Rigaku/MSC and Rigaku, 2000 ▶); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809049599/pk2211sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809049599/pk2211Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Co(C5H5N)2(H2O)4](C10H8ClN4O2S)2F(000) = 882
Mr = 856.62Dx = 1.536 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71070 Å
Hall symbol: -P 2ybcCell parameters from 6394 reflections
a = 8.5897 (12) Åθ = 3.1–27.5°
b = 25.807 (3) ŵ = 0.78 mm−1
c = 8.5338 (12) ÅT = 193 K
β = 101.694 (3)°Block, orange-yellow
V = 1852.5 (4) Å30.21 × 0.15 × 0.12 mm
Z = 2
Rigaku Mercury CCD diffractometer4226 independent reflections
Radiation source: fine-focus sealed tube3331 reflections with I > 2σ(I)
graphiteRint = 0.050
Detector resolution: 7.31 pixels mm-1θmax = 27.5°, θmin = 3.2°
ω scansh = −11→9
Absorption correction: multi-scan (REQAB; Jacobson, 1998)k = −32→33
Tmin = 0.853, Tmax = 0.912l = −10→11
20359 measured reflections
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.108H atoms treated by a mixture of independent and constrained refinement
S = 1.14w = 1/[σ2(Fo2) + (0.0291P)2 + 1.7941P] where P = (Fo2 + 2Fc2)/3
4226 reflections(Δ/σ)max < 0.001
258 parametersΔρmax = 0.66 e Å−3
1 restraintΔρmin = −0.44 e Å−3
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.
xyzUiso*/Ueq
Co11.00000.50000.50000.02572 (15)
Cl10.07781 (10)0.20506 (3)0.22874 (12)0.0489 (2)
S10.54834 (8)0.39936 (3)0.61366 (9)0.02737 (18)
O10.9392 (3)0.42160 (8)0.4313 (3)0.0348 (5)
O20.7795 (2)0.51495 (9)0.5400 (3)0.0337 (5)
O30.6620 (2)0.37878 (8)0.5233 (2)0.0330 (5)
O40.5622 (2)0.45443 (7)0.6462 (2)0.0331 (5)
N10.9177 (3)0.52499 (9)0.2536 (3)0.0315 (6)
N20.3692 (3)0.39029 (9)0.5297 (3)0.0299 (6)
N30.7205 (3)0.30830 (10)1.2615 (3)0.0394 (6)
H3A0.79670.28501.28270.047*
H3B0.67290.31901.33770.047*
N40.1620 (3)0.34401 (9)0.3915 (3)0.0309 (6)
N50.0921 (3)0.30070 (9)0.3205 (3)0.0323 (6)
C10.9858 (4)0.56332 (13)0.1875 (4)0.0405 (8)
H1C1.07050.58170.25300.049*
C20.9403 (4)0.57775 (15)0.0292 (4)0.0479 (9)
H2C0.99280.6054−0.01250.057*
C30.8187 (4)0.55177 (14)−0.0666 (4)0.0457 (9)
H30.78510.5609−0.17600.055*
C40.7458 (4)0.51210 (14)−0.0018 (4)0.0469 (9)
H40.66090.4933−0.06570.056*
C50.7977 (4)0.49995 (12)0.1575 (4)0.0378 (7)
H50.74630.47260.20150.045*
C60.5891 (3)0.36813 (10)0.8007 (3)0.0262 (6)
C70.7082 (4)0.33130 (12)0.8356 (4)0.0339 (7)
H70.76130.31990.75450.041*
C80.7499 (4)0.31125 (12)0.9877 (4)0.0355 (7)
H80.83070.28561.01010.043*
C90.6757 (3)0.32790 (11)1.1094 (3)0.0299 (6)
C100.5524 (4)0.36397 (12)1.0716 (4)0.0349 (7)
H100.49760.37501.15190.042*
C110.5097 (3)0.38357 (11)0.9191 (4)0.0334 (7)
H110.42520.40790.89460.040*
C120.3157 (3)0.34323 (11)0.4672 (3)0.0275 (6)
C130.1763 (3)0.25836 (11)0.3265 (4)0.0315 (7)
C140.3340 (4)0.25379 (11)0.4036 (4)0.0351 (7)
H140.38980.22190.40540.042*
C150.4049 (3)0.29672 (11)0.4761 (4)0.0328 (7)
H150.51240.29570.53210.039*
H1A0.859 (5)0.4089 (15)0.451 (5)0.060 (13)*
H1B1.005 (4)0.3990 (13)0.422 (4)0.038 (10)*
H2A0.717 (4)0.4932 (12)0.559 (5)0.070 (14)*
H2B0.734 (4)0.5420 (15)0.508 (5)0.058 (12)*
U11U22U33U12U13U23
Co10.0215 (3)0.0216 (3)0.0339 (3)0.0004 (2)0.0054 (2)−0.0016 (2)
Cl10.0384 (5)0.0396 (5)0.0696 (6)−0.0099 (3)0.0126 (4)−0.0209 (4)
S10.0224 (4)0.0263 (4)0.0332 (4)−0.0016 (3)0.0051 (3)0.0001 (3)
O10.0275 (12)0.0230 (11)0.0555 (15)−0.0012 (10)0.0120 (11)−0.0052 (10)
O20.0246 (11)0.0258 (12)0.0520 (14)0.0042 (9)0.0105 (10)0.0054 (10)
O30.0261 (11)0.0372 (11)0.0375 (12)−0.0036 (9)0.0105 (9)−0.0032 (9)
O40.0326 (11)0.0247 (10)0.0413 (12)−0.0052 (8)0.0061 (10)0.0010 (9)
N10.0284 (13)0.0287 (13)0.0373 (14)0.0042 (10)0.0063 (11)−0.0024 (11)
N20.0241 (13)0.0237 (12)0.0401 (14)0.0002 (9)0.0026 (11)0.0004 (11)
N30.0413 (16)0.0428 (15)0.0343 (14)0.0065 (12)0.0082 (12)0.0040 (12)
N40.0235 (12)0.0295 (13)0.0377 (14)0.0019 (10)0.0017 (11)−0.0023 (11)
N50.0261 (13)0.0296 (13)0.0399 (15)−0.0022 (10)0.0034 (11)−0.0043 (11)
C10.0365 (18)0.0438 (19)0.0411 (19)−0.0041 (14)0.0075 (15)0.0011 (15)
C20.049 (2)0.055 (2)0.041 (2)0.0012 (17)0.0155 (17)0.0091 (17)
C30.050 (2)0.056 (2)0.0301 (17)0.0174 (18)0.0056 (16)−0.0023 (16)
C40.046 (2)0.047 (2)0.042 (2)0.0085 (16)−0.0042 (17)−0.0120 (16)
C50.0353 (17)0.0331 (16)0.0422 (18)−0.0005 (13)0.0014 (15)−0.0027 (14)
C60.0198 (14)0.0253 (14)0.0334 (16)−0.0004 (11)0.0049 (12)0.0000 (12)
C70.0295 (16)0.0374 (17)0.0360 (17)0.0054 (13)0.0093 (14)−0.0033 (14)
C80.0316 (17)0.0368 (17)0.0379 (18)0.0097 (13)0.0063 (14)0.0014 (14)
C90.0294 (16)0.0269 (15)0.0325 (16)−0.0039 (12)0.0046 (13)−0.0014 (13)
C100.0341 (17)0.0353 (17)0.0390 (17)0.0016 (13)0.0159 (14)−0.0013 (14)
C110.0284 (16)0.0299 (16)0.0442 (18)0.0059 (12)0.0132 (14)−0.0003 (14)
C120.0245 (14)0.0260 (14)0.0318 (16)0.0021 (11)0.0053 (12)0.0017 (12)
C130.0270 (15)0.0292 (16)0.0394 (17)−0.0045 (12)0.0095 (13)−0.0053 (13)
C140.0293 (16)0.0250 (15)0.0505 (19)0.0052 (12)0.0070 (14)−0.0020 (14)
C150.0211 (15)0.0292 (15)0.0463 (18)0.0015 (11)0.0025 (13)0.0002 (14)
Co1—O2i2.028 (2)C1—C21.379 (5)
Co1—O22.028 (2)C1—H1C0.9500
Co1—O12.142 (2)C2—C31.365 (5)
Co1—O1i2.142 (2)C2—H2C0.9500
Co1—N1i2.176 (2)C3—C41.374 (5)
Co1—N12.176 (2)C3—H30.9500
Cl1—C131.737 (3)C4—C51.378 (5)
S1—O41.448 (2)C4—H40.9500
S1—O31.461 (2)C5—H50.9500
S1—N21.577 (2)C6—C71.384 (4)
S1—C61.759 (3)C6—C111.387 (4)
O1—H1A0.81 (4)C7—C81.376 (4)
O1—H1B0.83 (4)C7—H70.9500
O2—H2A0.82 (3)C8—C91.392 (4)
O2—H2B0.82 (4)C8—H80.9500
N1—C11.331 (4)C9—C101.398 (4)
N1—C51.346 (4)C10—C111.375 (4)
N2—C121.368 (3)C10—H100.9500
N3—C91.374 (4)C11—H110.9500
N3—H3A0.8800C12—C151.418 (4)
N3—H3B0.8800C13—C141.386 (4)
N4—C121.347 (4)C14—C151.352 (4)
N4—N51.352 (3)C14—H140.9500
N5—C131.306 (4)C15—H150.9500
O2i—Co1—O2180.0C1—C2—H2C120.5
O2i—Co1—O187.63 (9)C2—C3—C4118.8 (3)
O2—Co1—O192.37 (9)C2—C3—H3120.6
O2i—Co1—O1i92.37 (9)C4—C3—H3120.6
O2—Co1—O1i87.63 (9)C3—C4—C5119.0 (3)
O1—Co1—O1i180.00 (4)C3—C4—H4120.5
O2i—Co1—N1i88.56 (9)C5—C4—H4120.5
O2—Co1—N1i91.44 (9)N1—C5—C4123.1 (3)
O1—Co1—N1i89.87 (9)N1—C5—H5118.4
O1i—Co1—N1i90.13 (9)C4—C5—H5118.4
O2i—Co1—N191.44 (9)C7—C6—C11119.4 (3)
O2—Co1—N188.56 (9)C7—C6—S1120.8 (2)
O1—Co1—N190.13 (9)C11—C6—S1119.5 (2)
O1i—Co1—N189.87 (9)C8—C7—C6120.1 (3)
N1i—Co1—N1180.000 (1)C8—C7—H7120.0
O4—S1—O3114.83 (12)C6—C7—H7120.0
O4—S1—N2105.51 (12)C7—C8—C9121.1 (3)
O3—S1—N2113.63 (13)C7—C8—H8119.5
O4—S1—C6106.39 (13)C9—C8—H8119.5
O3—S1—C6106.34 (13)N3—C9—C8120.5 (3)
N2—S1—C6109.90 (13)N3—C9—C10121.1 (3)
Co1—O1—H1A120 (3)C8—C9—C10118.3 (3)
Co1—O1—H1B124 (2)C11—C10—C9120.5 (3)
H1A—O1—H1B111 (3)C11—C10—H10119.8
Co1—O2—H2A125 (3)C9—C10—H10119.8
Co1—O2—H2B120 (3)C10—C11—C6120.5 (3)
H2A—O2—H2B111 (4)C10—C11—H11119.7
C1—N1—C5116.5 (3)C6—C11—H11119.7
C1—N1—Co1123.0 (2)N4—C12—N2113.2 (2)
C5—N1—Co1120.4 (2)N4—C12—C15120.3 (3)
C12—N2—S1121.93 (19)N2—C12—C15126.5 (3)
C9—N3—H3A120.0N5—C13—C14124.8 (3)
C9—N3—H3B120.0N5—C13—Cl1115.6 (2)
H3A—N3—H3B120.0C14—C13—Cl1119.6 (2)
C12—N4—N5120.4 (2)C15—C14—C13117.0 (3)
C13—N5—N4118.8 (2)C15—C14—H14121.5
N1—C1—C2123.7 (3)C13—C14—H14121.5
N1—C1—H1C118.2C14—C15—C12118.7 (3)
C2—C1—H1C118.2C14—C15—H15120.6
C3—C2—C1119.0 (3)C12—C15—H15120.6
C3—C2—H2C120.5
O2i—Co1—N1—C1−57.6 (2)O3—S1—C6—C11173.7 (2)
O2—Co1—N1—C1122.4 (2)N2—S1—C6—C11−62.9 (3)
O1—Co1—N1—C1−145.2 (2)C11—C6—C7—C8−1.6 (4)
O1i—Co1—N1—C134.8 (2)S1—C6—C7—C8173.1 (2)
O2i—Co1—N1—C5119.1 (2)C6—C7—C8—C9−1.0 (5)
O2—Co1—N1—C5−60.9 (2)C7—C8—C9—N3−178.7 (3)
O1—Co1—N1—C531.5 (2)C7—C8—C9—C102.8 (5)
O1i—Co1—N1—C5−148.5 (2)N3—C9—C10—C11179.5 (3)
O4—S1—N2—C12173.4 (2)C8—C9—C10—C11−2.1 (4)
O3—S1—N2—C1246.8 (3)C9—C10—C11—C6−0.5 (5)
C6—S1—N2—C12−72.3 (3)C7—C6—C11—C102.3 (4)
C12—N4—N5—C13−0.2 (4)S1—C6—C11—C10−172.5 (2)
C5—N1—C1—C2−0.3 (5)N5—N4—C12—N2178.8 (2)
Co1—N1—C1—C2176.4 (3)N5—N4—C12—C15−1.3 (4)
N1—C1—C2—C30.1 (5)S1—N2—C12—N4−176.0 (2)
C1—C2—C3—C40.0 (5)S1—N2—C12—C154.2 (4)
C2—C3—C4—C50.1 (5)N4—N5—C13—C141.2 (5)
C1—N1—C5—C40.4 (5)N4—N5—C13—Cl1−178.8 (2)
Co1—N1—C5—C4−176.4 (2)N5—C13—C14—C15−0.7 (5)
C3—C4—C5—N1−0.3 (5)Cl1—C13—C14—C15179.3 (2)
O4—S1—C6—C7−123.9 (2)C13—C14—C15—C12−0.9 (5)
O3—S1—C6—C7−1.0 (3)N4—C12—C15—C141.8 (5)
N2—S1—C6—C7122.4 (2)N2—C12—C15—C14−178.3 (3)
O4—S1—C6—C1150.8 (3)
D—H···AD—HH···AD···AD—H···A
N3—H3A···N5ii0.882.523.135 (4)127
N3—H3B···O3iii0.882.233.001 (3)147
O1—H1A···O30.81 (4)2.07 (4)2.874 (3)174 (4)
O1—H1B···N4iv0.83 (4)2.01 (4)2.838 (3)178 (3)
O2—H2A···O40.82 (3)1.93 (4)2.726 (3)165 (4)
O2—H2B···N2v0.82 (4)1.96 (4)2.768 (3)170 (4)
O2—H2B···O4v0.82 (4)2.62 (4)3.142 (3)123 (3)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
N3—H3A⋯N5i 0.882.523.135 (4)127
N3—H3B⋯O3ii 0.882.233.001 (3)147
O1—H1A⋯O30.81 (4)2.07 (4)2.874 (3)174 (4)
O1—H1B⋯N4iii 0.83 (4)2.01 (4)2.838 (3)178 (3)
O2—H2A⋯O40.82 (3)1.93 (4)2.726 (3)165 (4)
O2—H2B⋯N2iv 0.82 (4)1.96 (4)2.768 (3)170 (4)
O2—H2B⋯O4iv 0.82 (4)2.62 (4)3.142 (3)123 (3)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) .

  1 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290
  1 in total
  1 in total

1.  Di-aqua-dichlorido-bis-(pyridine-κN)cobalt(II).

Authors:  P S Kannan; A S Ganeshraja; K Anbalagan; E Govindan; A Subbiahpandi
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2013-08-21
  1 in total

北京卡尤迪生物科技股份有限公司 © 2022-2023.