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The hydro­thermal reaction of cobalt acetate, vanadium pentoxide and 2,5-bis(4-pyridyl)-1,3,4-thia­diazo­le resulted in the title complex, [Co(V2O6)(C12H8N4S)(H2O)3], in which the cobalt(II) cation shows distorted octahedral geometry, coord­inated by one pyridine N atom, two O atoms from tetravanadate and three water mol­ecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804022111/hb6090sup1.cif
Contains datablocks I, co

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804022111/hb6090Isup2.hkl
Contains datablock I

CCDC reference: 252764

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.039
  • wR factor = 0.094
  • Data-to-parameter ratio = 13.3

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C12 H14 Co1 N4 O9 S1 V2 Atom count from _chemical_formula_moiety:
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 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 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-II (Johnson, 1976); software used to prepare material for publication: SHELXL97.

catena-poly[bis[cobalt(II)-2,5-bis(4-pyridyl) -1,3,4-thiadiazole](tetravanadate)(hexahydrate)] top
Crystal data top
[Co(C12H8N4S)(V2O6)3(H2O)]Z = 2
Mr = 551.14F(000) = 550
Triclinic, P1Dx = 2.001 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.0562 (18) ÅCell parameters from 86 reflections
b = 8.2506 (18) Åθ = 2.5–25.2°
c = 14.253 (3) ŵ = 2.07 mm1
α = 96.313 (3)°T = 293 K
β = 91.631 (3)°Block, red
γ = 103.402 (3)°0.28 × 0.21 × 0.12 mm
V = 914.6 (3) Å3
Data collection top
Bruker SMART Apex CCD Diffractometer3483 independent reflections
Radiation source: fine-focus sealed tube3035 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
φ and ω scansθmax = 26.0°, θmin = 1.4°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 89
Tmin = 0.595, Tmax = 0.789k = 107
4126 measured reflectionsl = 1417
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039Hydrogen site location: difmap (O-H) and geom (C-H)
wR(F2) = 0.094H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0485P)2]
where P = (Fo2 + 2Fc2)/3
3483 reflections(Δ/σ)max < 0.001
262 parametersΔρmax = 0.55 e Å3
0 restraintsΔρmin = 0.40 e Å3
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
xyzUiso*/Ueq
Co10.23745 (6)0.15653 (5)0.38131 (3)0.01374 (14)
V10.09244 (7)0.25405 (7)0.46779 (4)0.01310 (15)
V20.19563 (7)0.43253 (7)0.64109 (4)0.01500 (16)
S10.68596 (12)0.41363 (11)0.12653 (6)0.0197 (2)
N10.4249 (4)0.0801 (3)0.29940 (18)0.0148 (6)
N20.6583 (4)0.1980 (4)0.0162 (2)0.0224 (7)
N30.7116 (4)0.3198 (4)0.0381 (2)0.0217 (7)
C110.8823 (5)0.8395 (4)0.0293 (3)0.0232 (8)
H11A0.90490.92470.00660.080*
O10.1785 (3)0.0811 (3)0.42268 (15)0.0190 (5)
O20.0650 (3)0.2329 (3)0.53529 (15)0.0199 (6)
O30.2475 (3)0.3182 (3)0.53858 (16)0.0186 (5)
O40.3511 (3)0.5304 (3)0.65283 (16)0.0204 (6)
O50.1903 (3)0.3036 (3)0.73515 (16)0.0218 (6)
O60.0145 (3)0.5768 (3)0.62458 (15)0.0177 (5)
C10.5054 (5)0.0304 (4)0.3291 (2)0.0195 (8)
H1A0.50730.04230.39530.080*
C20.5852 (5)0.1293 (4)0.2702 (2)0.0191 (8)
H2A0.64350.20610.29470.080*
C30.5805 (4)0.1132 (4)0.1739 (2)0.0167 (7)
C40.5083 (5)0.0112 (4)0.1437 (2)0.0189 (8)
H4A0.51220.03220.07870.080*
C50.4323 (4)0.1039 (4)0.2075 (2)0.0181 (8)
H5A0.38220.18890.18570.080*
C60.6413 (4)0.2272 (4)0.1041 (2)0.0178 (8)
C70.7318 (4)0.4413 (4)0.0088 (2)0.0179 (8)
C80.7913 (5)0.5854 (4)0.0348 (2)0.0187 (8)
C90.8209 (5)0.5973 (4)0.1313 (2)0.0213 (8)
H9A0.80150.51360.16930.080*
C100.8787 (5)0.7333 (5)0.1701 (3)0.0241 (9)
H10A0.89660.74320.23650.080*
N40.9109 (4)0.8529 (4)0.1214 (2)0.0228 (7)
C120.8231 (5)0.7097 (4)0.0169 (2)0.0204 (8)
H12A0.80370.70520.08320.080*
O1W0.4151 (3)0.2473 (3)0.49621 (16)0.0200 (5)
O2W0.0464 (3)0.0856 (3)0.27223 (17)0.0247 (6)
O3W0.2934 (3)0.3962 (3)0.33170 (16)0.0215 (6)
H3WA0.40750.44620.34310.050*
H1WA0.52750.28060.48770.050*
H3WB0.24390.47170.35570.050*
H2WA0.05230.03540.22070.050*
H2WB0.02560.15440.26740.050*
H1WB0.38910.32400.54400.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0152 (3)0.0119 (3)0.0140 (2)0.00247 (19)0.00297 (18)0.00214 (18)
V10.0139 (3)0.0109 (3)0.0143 (3)0.0020 (2)0.0026 (2)0.0024 (2)
V20.0159 (3)0.0138 (3)0.0151 (3)0.0026 (2)0.0012 (2)0.0023 (2)
S10.0274 (5)0.0179 (5)0.0159 (4)0.0091 (4)0.0038 (4)0.0021 (3)
N10.0167 (16)0.0144 (15)0.0138 (14)0.0034 (12)0.0035 (12)0.0034 (11)
N20.0313 (19)0.0206 (17)0.0188 (16)0.0113 (14)0.0070 (13)0.0047 (13)
N30.0297 (19)0.0223 (17)0.0158 (15)0.0113 (14)0.0039 (13)0.0025 (13)
C110.021 (2)0.0169 (19)0.031 (2)0.0034 (15)0.0032 (16)0.0031 (16)
O10.0231 (14)0.0131 (12)0.0207 (13)0.0021 (10)0.0033 (11)0.0055 (10)
O20.0207 (14)0.0207 (13)0.0181 (13)0.0046 (11)0.0041 (10)0.0012 (10)
O30.0168 (13)0.0189 (13)0.0217 (13)0.0038 (10)0.0020 (10)0.0097 (10)
O40.0210 (14)0.0199 (13)0.0222 (13)0.0070 (11)0.0013 (11)0.0056 (10)
O50.0257 (15)0.0196 (14)0.0183 (13)0.0038 (11)0.0009 (11)0.0027 (10)
O60.0205 (14)0.0145 (12)0.0154 (12)0.0001 (10)0.0007 (10)0.0000 (9)
C10.022 (2)0.0179 (19)0.0195 (19)0.0047 (15)0.0029 (15)0.0052 (15)
C20.023 (2)0.0186 (19)0.0181 (18)0.0074 (15)0.0026 (15)0.0064 (15)
C30.0153 (19)0.0128 (17)0.0206 (18)0.0016 (14)0.0023 (14)0.0006 (14)
C40.020 (2)0.0192 (19)0.0170 (18)0.0038 (15)0.0038 (15)0.0043 (14)
C50.020 (2)0.0159 (18)0.0179 (18)0.0026 (15)0.0029 (15)0.0036 (14)
C60.0140 (19)0.0182 (19)0.0208 (19)0.0024 (14)0.0002 (14)0.0041 (14)
C70.0184 (19)0.0199 (19)0.0145 (17)0.0041 (15)0.0008 (14)0.0012 (14)
C80.019 (2)0.0160 (18)0.0202 (18)0.0029 (15)0.0011 (15)0.0010 (14)
C90.022 (2)0.022 (2)0.0195 (19)0.0062 (16)0.0012 (15)0.0013 (15)
C100.025 (2)0.022 (2)0.023 (2)0.0040 (16)0.0053 (16)0.0031 (16)
N40.0216 (18)0.0184 (17)0.0256 (17)0.0026 (13)0.0020 (13)0.0049 (13)
C120.022 (2)0.0193 (19)0.0187 (18)0.0028 (15)0.0008 (15)0.0021 (15)
O1W0.0167 (14)0.0243 (14)0.0175 (12)0.0027 (10)0.0009 (10)0.0004 (10)
O2W0.0276 (16)0.0248 (14)0.0222 (13)0.0124 (12)0.0063 (11)0.0062 (11)
O3W0.0241 (15)0.0155 (13)0.0254 (13)0.0052 (11)0.0041 (11)0.0035 (10)
Geometric parameters (Å, º) top
Co1—O2i2.019 (2)O6—V1ii1.794 (2)
Co1—O12.063 (2)C1—C21.380 (5)
Co1—O2W2.092 (2)C1—H1A0.9600
Co1—O1W2.096 (2)C2—C31.395 (5)
Co1—N12.102 (3)C2—H2A0.9600
Co1—O3W2.127 (2)C3—C41.391 (5)
V1—O11.643 (2)C3—C61.466 (5)
V1—O21.643 (2)C4—C51.372 (5)
V1—O31.792 (2)C4—H4A0.9599
V1—O6ii1.794 (2)C5—H5A0.9601
V2—O51.625 (2)C7—C81.465 (5)
V2—O41.654 (2)C8—C121.392 (5)
V2—O61.822 (2)C8—C91.400 (5)
V2—O31.831 (2)C9—C101.379 (5)
S1—C61.719 (4)C9—H9A0.9599
S1—C71.730 (3)C10—N41.335 (5)
N1—C11.332 (4)C10—H10A0.9600
N1—C51.347 (4)C12—H12A0.9599
N2—C61.306 (4)O1W—H1WA0.8991
N2—N31.357 (4)O1W—H1WB0.9391
N3—C71.303 (4)O2W—H2WA0.8111
C11—N41.337 (5)O2W—H2WB0.9063
C11—C121.381 (5)O3W—H3WA0.9176
C11—H11A0.9600O3W—H3WB0.8606
O2—Co1i2.019 (2)
O2i—Co1—O192.51 (9)C2—C1—H1A118.2
O2i—Co1—O2W88.19 (10)C1—C2—C3118.1 (3)
O1—Co1—O2W91.26 (10)C1—C2—H2A121.2
O2i—Co1—O1W86.38 (10)C3—C2—H2A120.7
O1—Co1—O1W91.95 (9)C4—C3—C2118.1 (3)
O2W—Co1—O1W173.81 (9)C4—C3—C6119.6 (3)
O2i—Co1—N1177.54 (10)C2—C3—C6122.2 (3)
O1—Co1—N187.41 (10)C5—C4—C3119.5 (3)
O2W—Co1—N194.27 (10)C5—C4—H4A120.3
O1W—Co1—N191.16 (10)C3—C4—H4A120.2
O2i—Co1—O3W88.71 (9)N1—C5—C4122.5 (3)
O1—Co1—O3W177.14 (9)N1—C5—H5A118.7
O2W—Co1—O3W86.19 (10)C4—C5—H5A118.7
O1W—Co1—O3W90.71 (9)N2—C6—C3121.7 (3)
N1—Co1—O3W91.48 (10)N2—C6—S1113.7 (3)
O1—V1—O2112.63 (12)C3—C6—S1124.5 (3)
O1—V1—O3111.07 (12)N3—C7—C8122.4 (3)
O2—V1—O3107.25 (11)N3—C7—S1113.7 (3)
O1—V1—O6ii110.37 (11)C8—C7—S1123.9 (3)
O2—V1—O6ii108.94 (12)C12—C8—C9118.5 (3)
O3—V1—O6ii106.32 (11)C12—C8—C7122.3 (3)
O5—V2—O4110.76 (13)C9—C8—C7119.1 (3)
O5—V2—O6106.41 (12)C10—C9—C8117.8 (3)
O4—V2—O6112.50 (12)C10—C9—H9A121.1
O5—V2—O3110.72 (12)C8—C9—H9A121.1
O4—V2—O3104.82 (11)N4—C10—C9124.4 (3)
O6—V2—O3111.72 (11)N4—C10—H10A117.6
C6—S1—C786.83 (17)C9—C10—H10A118.0
C1—N1—C5117.5 (3)C10—N4—C11117.0 (3)
C1—N1—Co1119.8 (2)C11—C12—C8118.6 (3)
C5—N1—Co1120.3 (2)C11—C12—H12A120.9
C6—N2—N3113.1 (3)C8—C12—H12A120.5
C7—N3—N2112.7 (3)Co1—O1W—H1WA121.3
N4—C11—C12123.6 (3)Co1—O1W—H1WB118.1
N4—C11—H11A117.9H1WA—O1W—H1WB107.1
C12—C11—H11A118.5Co1—O2W—H2WA127.0
V1—O1—Co1165.77 (15)Co1—O2W—H2WB116.8
V1—O2—Co1i168.36 (15)H2WA—O2W—H2WB109.3
V1—O3—V2123.74 (13)Co1—O3W—H3WA109.9
V1ii—O6—V2128.55 (13)Co1—O3W—H3WB119.0
N1—C1—C2123.9 (3)H3WA—O3W—H3WB103.3
N1—C1—H1A117.9
O1—Co1—N1—C132.6 (3)C1—C2—C3—C45.3 (5)
O2W—Co1—N1—C1123.7 (3)C1—C2—C3—C6171.8 (3)
O1W—Co1—N1—C159.3 (3)C2—C3—C4—C55.3 (5)
O3W—Co1—N1—C1150.0 (3)C6—C3—C4—C5171.9 (3)
O1—Co1—N1—C5129.2 (3)C1—N1—C5—C44.6 (5)
O2W—Co1—N1—C538.1 (3)Co1—N1—C5—C4157.6 (3)
O1W—Co1—N1—C5138.9 (3)C3—C4—C5—N10.3 (5)
O3W—Co1—N1—C548.2 (3)N3—N2—C6—C3178.3 (3)
C6—N2—N3—C71.0 (4)N3—N2—C6—S11.4 (4)
O2—V1—O1—Co16.3 (6)C4—C3—C6—N212.4 (5)
O3—V1—O1—Co1126.6 (6)C2—C3—C6—N2170.5 (3)
O6ii—V1—O1—Co1115.7 (6)C4—C3—C6—S1164.1 (3)
O2i—Co1—O1—V19.7 (6)C2—C3—C6—S113.0 (5)
O2W—Co1—O1—V178.5 (6)C7—S1—C6—N21.1 (3)
O1W—Co1—O1—V196.2 (6)C7—S1—C6—C3177.9 (3)
N1—Co1—O1—V1172.7 (6)N2—N3—C7—C8179.0 (3)
O1—V1—O2—Co1i18.0 (8)N2—N3—C7—S10.1 (4)
O3—V1—O2—Co1i104.5 (7)C6—S1—C7—N30.5 (3)
O6ii—V1—O2—Co1i140.8 (7)C6—S1—C7—C8178.3 (3)
O1—V1—O3—V2149.75 (14)N3—C7—C8—C12175.9 (3)
O2—V1—O3—V226.29 (19)S1—C7—C8—C122.9 (5)
O6ii—V1—O3—V290.15 (16)N3—C7—C8—C92.7 (5)
O5—V2—O3—V184.03 (18)S1—C7—C8—C9178.5 (3)
O4—V2—O3—V1156.50 (15)C12—C8—C9—C100.6 (5)
O6—V2—O3—V134.39 (19)C7—C8—C9—C10179.2 (3)
O5—V2—O6—V1ii178.61 (16)C8—C9—C10—N41.1 (6)
O4—V2—O6—V1ii59.93 (19)C9—C10—N4—C111.0 (6)
O3—V2—O6—V1ii57.65 (19)C12—C11—N4—C100.4 (5)
C5—N1—C1—C24.6 (5)N4—C11—C12—C80.1 (6)
Co1—N1—C1—C2157.7 (3)C9—C8—C12—C110.1 (5)
N1—C1—C2—C30.4 (5)C7—C8—C12—C11178.7 (3)
Symmetry codes: (i) x, y, z+1; (ii) x, y1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O3W—H3WA···O4iii0.921.902.813 (3)171
O1W—H1WA···O3iii0.901.822.716 (3)172
O3W—H3WB···O6i0.862.233.014 (3)152
O2W—H2WA···N4iv0.812.032.804 (4)160
O2W—H2WB···O5i0.912.012.916 (3)176
O1W—H1WB···O4v0.941.932.867 (3)173
Symmetry codes: (i) x, y, z+1; (iii) x+1, y, z+1; (iv) x+1, y1, z; (v) x, y+1, z.
 

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