Literature DB >> 21583739

Tetra-aqua-bis(3,5-di-4-pyridyl-1,2,4-triazolato-κN)cobalt(II) dihydrate.

Lin Yi Dong1.   

Abstract

The Co(II) atom in the title compound, [Co(C(12)H(8)N(5))(2)(H(2)O)(4)]·2H(2)O, lies on a center of inversion and is bonded to two N-heterocycles and to four water mol-ecules in a slightly distorted octahedral coordination. The coordinated and lattice water mol-ecules inter-act with the N-heterocycles through O-H⋯N hydrogen bonds, generating a three-dimensional supra-molecular architecture.

Entities:  

Year:  2009        PMID： 21583739      PMCID： PMC2977553          DOI： 10.1107/S1600536809011982

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


Related literature

For magnetic studies of transition metal complexes with 1,2,4-triazole derivatives, see: Haasnoot (2000 ▶). For the potential applications of complexes containing substituted 1,2,4-triazole ligands with spin-crossover properties in mol­ecular-based memory devices, displays and optical switches, see: Kahn & Martinez (1998 ▶). For 3,5-di(4-pyridine)-1,2,4-triazole, see: Zhang et al. (2006 ▶); Sreenivasulu & Vittal (2004 ▶). For the structure of water, see: Tajkhorshid et al. (2002 ▶). For the synthesis, see: Basu & Dutta (1964 ▶). For a trinuclear water cluster, see: König (1944 ▶).

Experimental

Crystal data

[Co(C12H8N5)2(H2O)4]·2H2O M = 611.49 Monoclinic, a = 7.3660 (15) Å b = 15.654 (3) Å c = 11.857 (2) Å β = 107.34 (3)° V = 1305.1 (5) Å3 Z = 2 Mo Kα radiation μ = 0.72 mm−1 T = 293 K 0.40 × 0.20 × 0.12 mm

Data collection

Bruker SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.842, T max = 0.917 11054 measured reflections 2423 independent reflections 2009 reflections with I > 2σ(I) R int = 0.065

Refinement

R[F 2 > 2σ(F 2)] = 0.054 wR(F 2) = 0.108 S = 1.07 2420 reflections 243 parameters H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.29 e Å−3 Δρmin = −0.41 e Å−3 Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXL97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: publCIF (Westrip, 2009 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809011982/ng2566sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809011982/ng2566Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Co(C12H8N5)2(H2O)4]·2(H2O)F(000) = 634
Mr = 611.49Dx = 1.556 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 556 reflections
a = 7.3660 (15) Åθ = 1.5–25.5°
b = 15.654 (3) ŵ = 0.72 mm−1
c = 11.857 (2) ÅT = 293 K
β = 107.34 (3)°Block, red
V = 1305.1 (5) Å30.40 × 0.20 × 0.12 mm
Z = 2
Bruker SMART CCD area-detector diffractometer2423 independent reflections
Radiation source: fine-focus sealed tube2009 reflections with I > 2σ(I)
graphiteRint = 0.065
φ and ω scansθmax = 25.5°, θmin = 3.2°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −8→8
Tmin = 0.842, Tmax = 0.917k = −18→18
11054 measured reflectionsl = −14→14
Refinement on F20 restraints
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.054w = 1/[σ2(Fo2) + (0.0298P)2 + 0.2298P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.108(Δ/σ)max < 0.001
S = 1.07Δρmax = 0.29 e Å−3
2420 reflectionsΔρmin = −0.41 e Å−3
243 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.
xyzUiso*/Ueq
C10.3827 (5)0.6826 (2)−0.0776 (3)0.0306 (8)
C20.3536 (5)0.7690 (2)−0.0713 (3)0.0299 (8)
C30.3919 (4)0.80864 (19)0.0377 (3)0.0218 (7)
C40.4634 (5)0.7565 (2)0.1360 (3)0.0290 (8)
C50.4886 (5)0.6711 (2)0.1224 (3)0.0294 (8)
C60.3518 (5)0.8987 (2)0.0514 (3)0.0229 (7)
C70.2496 (5)1.02433 (19)0.0220 (3)0.0241 (7)
C80.1690 (5)1.1049 (2)−0.0324 (3)0.0244 (7)
C90.1117 (5)1.1170 (2)−0.1528 (3)0.0330 (9)
C100.0440 (6)1.1952 (2)−0.1990 (3)0.0368 (9)
C110.0861 (6)1.2510 (3)−0.0181 (4)0.0450 (11)
C120.1540 (6)1.1751 (2)0.0357 (4)0.0403 (10)
Co10.50000.50000.00000.02203 (19)
H10.363 (5)0.657 (2)−0.147 (3)0.033 (10)*
H20.313 (5)0.799 (3)−0.138 (3)0.046 (12)*
H40.495 (5)0.781 (2)0.209 (3)0.034 (10)*
H50.532 (5)0.637 (2)0.187 (3)0.036 (10)*
H90.118 (5)1.075 (2)−0.199 (3)0.028 (10)*
H100.013 (6)1.203 (3)−0.278 (4)0.052 (13)*
H110.078 (6)1.299 (3)0.026 (4)0.057 (13)*
H120.188 (6)1.170 (3)0.116 (4)0.051 (12)*
H1A0.261 (5)0.484 (3)−0.2116 (18)0.069 (16)*
H2A0.276 (4)0.5057 (16)0.135 (3)0.031 (10)*
H3A0.163 (5)0.571 (2)0.2816 (10)0.041 (12)*
H1B0.143 (3)0.475 (3)−0.140 (3)0.077 (17)*
H2B0.416 (6)0.446 (3)0.1861 (19)0.084 (18)*
H3B0.081 (6)0.6269 (11)0.194 (4)0.069 (16)*
N10.4483 (4)0.63277 (16)0.0175 (2)0.0262 (6)
N20.2624 (4)0.95193 (16)−0.0378 (2)0.0229 (6)
N30.3929 (4)0.93481 (17)0.1575 (2)0.0295 (7)
N40.3253 (4)1.01645 (17)0.1389 (2)0.0308 (7)
N50.0298 (4)1.26290 (18)−0.1346 (3)0.0371 (8)
O10.2504 (3)0.49368 (17)−0.1431 (2)0.0334 (6)
O20.3487 (4)0.46767 (16)0.1212 (2)0.0302 (6)
O30.1157 (4)0.57516 (16)0.2069 (2)0.0329 (6)
U11U22U33U12U13U23
C10.047 (2)0.0220 (18)0.0201 (18)0.0038 (16)0.0054 (16)−0.0033 (15)
C20.044 (2)0.0184 (17)0.0245 (19)0.0057 (15)0.0057 (16)0.0020 (15)
C30.0241 (18)0.0184 (16)0.0231 (17)0.0017 (13)0.0074 (14)−0.0003 (13)
C40.043 (2)0.0239 (18)0.0188 (18)0.0052 (16)0.0075 (16)−0.0032 (15)
C50.043 (2)0.0200 (18)0.0232 (19)0.0050 (15)0.0065 (16)0.0043 (14)
C60.0277 (18)0.0182 (16)0.0224 (17)−0.0006 (14)0.0066 (14)0.0000 (13)
C70.0297 (18)0.0194 (17)0.0227 (17)−0.0001 (13)0.0072 (14)0.0002 (13)
C80.0247 (18)0.0211 (17)0.0269 (18)−0.0023 (14)0.0067 (14)−0.0009 (14)
C90.044 (2)0.0231 (19)0.028 (2)0.0046 (16)0.0043 (17)−0.0031 (16)
C100.044 (2)0.033 (2)0.027 (2)0.0034 (17)0.0023 (18)0.0073 (17)
C110.067 (3)0.024 (2)0.045 (3)0.013 (2)0.017 (2)−0.0019 (18)
C120.065 (3)0.027 (2)0.028 (2)0.0129 (18)0.011 (2)0.0002 (16)
Co10.0282 (4)0.0162 (3)0.0206 (3)0.0025 (3)0.0055 (2)0.0004 (3)
N10.0358 (17)0.0170 (14)0.0251 (15)0.0032 (12)0.0081 (12)−0.0001 (11)
N20.0283 (15)0.0154 (14)0.0241 (15)0.0011 (11)0.0063 (12)−0.0011 (11)
N30.0398 (18)0.0213 (15)0.0255 (16)0.0099 (13)0.0065 (13)0.0017 (12)
N40.0461 (18)0.0213 (16)0.0221 (15)0.0069 (13)0.0057 (13)−0.0013 (11)
N50.044 (2)0.0223 (16)0.044 (2)0.0079 (14)0.0115 (16)0.0055 (14)
O10.0312 (14)0.0408 (15)0.0264 (14)−0.0029 (13)0.0058 (10)−0.0009 (12)
O20.0346 (15)0.0295 (13)0.0296 (14)0.0062 (11)0.0142 (12)0.0021 (11)
O30.0436 (16)0.0239 (14)0.0286 (15)0.0017 (12)0.0067 (12)0.0018 (11)
C1—N11.337 (4)C10—N51.328 (5)
C1—C21.376 (5)C10—H100.90 (4)
C1—H10.89 (4)C11—N51.331 (5)
C2—C31.385 (5)C11—C121.370 (5)
C2—H20.89 (4)C11—H110.93 (4)
C3—C41.392 (5)C12—H120.92 (4)
C3—C61.459 (4)Co1—O1i2.100 (2)
C4—C51.365 (5)Co1—O12.100 (2)
C4—H40.91 (4)Co1—O2i2.126 (2)
C5—N11.332 (4)Co1—O22.126 (2)
C5—H50.91 (4)Co1—N1i2.134 (3)
C6—N31.329 (4)Co1—N12.134 (3)
C6—N21.354 (4)N3—N41.365 (4)
C7—N41.336 (4)O1—H1A0.851 (10)
C7—N21.355 (4)O1—H1B0.852 (10)
C7—C81.459 (4)O2—H2A0.851 (10)
C8—C91.377 (5)O2—H2B0.850 (10)
C8—C121.387 (5)O3—H3A0.852 (10)
C9—C101.373 (5)O3—H3B0.849 (10)
C9—H90.87 (4)
N1—C1—C2123.4 (3)C11—C12—C8119.8 (4)
N1—C1—H1116 (2)C11—C12—H12121 (3)
C2—C1—H1121 (2)C8—C12—H12120 (3)
C1—C2—C3120.0 (3)O1i—Co1—O1180.0
C1—C2—H2119 (3)O1i—Co1—O2i91.47 (10)
C3—C2—H2121 (3)O1—Co1—O2i88.53 (10)
C2—C3—C4116.1 (3)O1i—Co1—O288.53 (10)
C2—C3—C6123.0 (3)O1—Co1—O291.47 (10)
C4—C3—C6120.8 (3)O2i—Co1—O2180.0
C5—C4—C3120.4 (3)O1i—Co1—N1i89.19 (10)
C5—C4—H4122 (2)O1—Co1—N1i90.81 (10)
C3—C4—H4118 (2)O2i—Co1—N1i91.23 (10)
N1—C5—C4123.5 (3)O2—Co1—N1i88.77 (10)
N1—C5—H5116 (2)O1i—Co1—N190.81 (10)
C4—C5—H5120 (2)O1—Co1—N189.19 (10)
N3—C6—N2113.4 (3)O2i—Co1—N188.77 (10)
N3—C6—C3121.3 (3)O2—Co1—N191.23 (10)
N2—C6—C3125.1 (3)N1i—Co1—N1180.0
N4—C7—N2113.1 (3)C5—N1—C1116.7 (3)
N4—C7—C8121.8 (3)C5—N1—Co1122.2 (2)
N2—C7—C8125.0 (3)C1—N1—Co1121.0 (2)
C9—C8—C12116.1 (3)C6—N2—C7101.5 (3)
C9—C8—C7122.5 (3)C6—N3—N4106.0 (2)
C12—C8—C7121.3 (3)C7—N4—N3105.8 (2)
C10—C9—C8120.0 (3)C10—N5—C11115.6 (3)
C10—C9—H9120 (2)Co1—O1—H1A118 (3)
C8—C9—H9120 (2)Co1—O1—H1B126 (3)
N5—C10—C9124.3 (4)H1A—O1—H1B109.1 (17)
N5—C10—H10117 (3)Co1—O2—H2A117 (2)
C9—C10—H10119 (3)Co1—O2—H2B115 (3)
N5—C11—C12124.2 (4)H2A—O2—H2B109.4 (15)
N5—C11—H11115 (3)H3A—O3—H3B106 (4)
C12—C11—H11121 (3)
N1—C1—C2—C3−0.3 (6)C2—C1—N1—Co1−177.5 (3)
C1—C2—C3—C41.4 (5)O1i—Co1—N1—C5−36.4 (3)
C1—C2—C3—C6−175.5 (3)O1—Co1—N1—C5143.6 (3)
C2—C3—C4—C5−1.3 (5)O2i—Co1—N1—C5−127.9 (3)
C6—C3—C4—C5175.6 (3)O2—Co1—N1—C552.1 (3)
C3—C4—C5—N10.1 (6)N1i—Co1—N1—C5−122 (27)
C2—C3—C6—N3−179.1 (3)O1i—Co1—N1—C1140.0 (3)
C4—C3—C6—N34.2 (5)O1—Co1—N1—C1−40.0 (3)
C2—C3—C6—N24.7 (5)O2i—Co1—N1—C148.5 (3)
C4—C3—C6—N2−172.0 (3)O2—Co1—N1—C1−131.5 (3)
N4—C7—C8—C9171.9 (3)N1i—Co1—N1—C155 (27)
N2—C7—C8—C9−5.8 (5)N3—C6—N2—C7−0.6 (4)
N4—C7—C8—C12−5.0 (5)C3—C6—N2—C7175.9 (3)
N2—C7—C8—C12177.3 (3)N4—C7—N2—C60.0 (4)
C12—C8—C9—C10−0.2 (6)C8—C7—N2—C6177.9 (3)
C7—C8—C9—C10−177.4 (3)N2—C6—N3—N40.8 (4)
C8—C9—C10—N50.5 (6)C3—C6—N3—N4−175.7 (3)
N5—C11—C12—C80.6 (7)N2—C7—N4—N30.5 (4)
C9—C8—C12—C11−0.3 (6)C8—C7—N4—N3−177.5 (3)
C7—C8—C12—C11176.9 (4)C6—N3—N4—C7−0.8 (4)
C4—C5—N1—C11.1 (5)C9—C10—N5—C11−0.2 (6)
C4—C5—N1—Co1177.6 (3)C12—C11—N5—C10−0.3 (6)
C2—C1—N1—C5−1.0 (5)
D—H···AD—HH···AD···AD—H···A
O1—H1A···N3ii0.85 (1)2.42 (3)3.070 (4)134 (3)
O1—H1A···N4ii0.85 (1)1.97 (1)2.803 (4)167 (4)
O1—H1B···O3iii0.85 (1)1.99 (2)2.791 (4)155 (3)
O2—H2A···O30.85 (1)1.97 (1)2.801 (4)164 (3)
O2—H2B···N3iv0.85 (1)1.97 (2)2.792 (4)161 (5)
O2—H2B···N4iv0.85 (1)2.60 (4)3.220 (4)130 (4)
O3—H3A···N2v0.85 (1)2.08 (1)2.926 (4)174 (4)
O3—H3B···N5vi0.85 (1)1.95 (1)2.786 (4)168 (5)
Table 1

Selected geometric parameters (Å, °)

Co1—O12.100 (2)
Co1—O22.126 (2)
Co1—N12.134 (3)
Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O1—H1A⋯N3ii0.851 (10)2.42 (3)3.070 (4)134 (3)
O1—H1A⋯N4ii0.851 (10)1.966 (12)2.803 (4)167 (4)
O1—H1B⋯O3iii0.852 (10)1.99 (2)2.791 (4)155 (3)
O2—H2A⋯O30.851 (10)1.973 (14)2.801 (4)164 (3)
O2—H2B⋯N3iv0.850 (10)1.973 (19)2.792 (4)161 (5)
O2—H2B⋯N4iv0.850 (10)2.60 (4)3.220 (4)130 (4)
O3—H3A⋯N2v0.852 (10)2.077 (12)2.926 (4)174 (4)
O3—H3B⋯N5vi0.849 (10)1.950 (14)2.786 (4)168 (5)

Symmetry codes: (ii) ; (iii) ; (iv) ; (v) ; (vi) .

  4 in total

1.  Control of the selectivity of the aquaporin water channel family by global orientational tuning.

Authors:  Emad Tajkhorshid; Peter Nollert; Morten Ø Jensen; Larry J W Miercke; Joseph O'Connell; Robert M Stroud; Klaus Schulten
Journal:  Science       Date:  2002-04-19       Impact factor: 47.728

2.  Helix inside a Helix: encapsulation of hydrogen-bonded water molecules in a staircase coordination polymer.

Authors:  Bellam Sreenivasulu; Jagadese J Vittal
Journal:  Angew Chem Int Ed Engl       Date:  2004-11-05       Impact factor: 15.336

3.  A short history of SHELX.

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

4.  Abnormal products during isolation of isonicotinic acid hydrazide.

Authors:  U P Basu; S Dutta
Journal:  J Org Chem       Date:  1965-10       Impact factor: 4.354
  4 in total
  1 in total

1.  Diaqua-bis-(3-nitro-benzoato-κO)bis-[1H-5-(3-pyrid-yl)-3-(4-pyrid-yl)-1H-1,2,4-triazole-κN]cobalt(II) dihydrate.

Authors:  Yun-Liang Zhang; Ti-Lou Liu; Shuang-Jiao Sun; Jie-Hong Li; Shi-Qing Wu
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-11-17
  1 in total

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