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The mol­ecule of the title compound, [{Cd(bpy)2}2V4O12] (bpy is 2,2′-bi­pyridine) or [Cd2V4O12(C10H8N2)4], has crystallographic twofold rotation symmetry. A {V4O12} ring links through oxo groups of pairs of adjacent vanadium sites to two {Cd(bpy)2} moieties. The mol­ecules are assembled into layers parallel to the ab plane by aromatic π–π stacking interactions involving the bpy ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680401623X/cf6361sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680401623X/cf6361Isup2.hkl
Contains datablock I

CCDC reference: 248728

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.017 Å
  • R factor = 0.071
  • wR factor = 0.210
  • Data-to-parameter ratio = 15.7

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... O3 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... O4 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... O5 PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C11 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... V1 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... V2 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 17 PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C15 - C16 ... 1.53 Ang.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 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 7 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

Computing details top

Data collection: R3m Software (Siemens, 1990); cell refinement: R3m Software; data reduction: R3m Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 1998); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
[Cd2V4O12(C10H8N2)4]F(000) = 4896
Mr = 1245.30Dx = 1.733 Mg m3
Orthorhombic, IbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -I 2b 2cCell parameters from 25 reflections
a = 16.287 (7) Åθ = 2–26°
b = 17.201 (9) ŵ = 1.69 mm1
c = 34.070 (16) ÅT = 293 K
V = 9545 (8) Å3Block, brown
Z = 80.20 × 0.18 × 0.12 mm
Data collection top
Siemens R3m
diffractometer
2729 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.074
Graphite monochromatorθmax = 26.0°, θmin = 2.1°
ω scansh = 020
Absorption correction: ψ scan
(North et al., 1968)
k = 021
Tmin = 0.728, Tmax = 0.823l = 142
4865 measured reflections2 standard reflections every 200 reflections
4707 independent reflections intensity decay: none
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.071H-atom parameters constrained
wR(F2) = 0.210 w = 1/[σ2(Fo2) + (0.1212P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.001
4707 reflectionsΔρmax = 1.02 e Å3
300 parametersΔρmin = 0.95 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00085 (10)
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
Cd10.76193 (4)0.22365 (4)0.122200 (19)0.0436 (3)
V10.56374 (9)0.16781 (9)0.16295 (5)0.0416 (4)
V20.57714 (9)0.18058 (9)0.06668 (5)0.0451 (4)
N10.8166 (4)0.1062 (5)0.0966 (2)0.051 (2)
N20.8595 (5)0.1700 (5)0.1676 (2)0.054 (2)
N30.8493 (6)0.3091 (5)0.0868 (3)0.065 (2)
N40.7595 (5)0.3486 (5)0.1515 (2)0.054 (2)
O10.50000.25000.1737 (4)0.082 (4)
O20.5407 (4)0.0972 (4)0.1932 (2)0.065 (2)
O30.6636 (4)0.1891 (4)0.1680 (2)0.0600 (18)
O40.5483 (4)0.1342 (4)0.11307 (19)0.0598 (18)
O50.6675 (4)0.2230 (4)0.0728 (2)0.065 (2)
O60.5859 (5)0.1145 (4)0.0330 (2)0.074 (2)
O70.50000.25000.0523 (3)0.065 (3)
C10.7925 (7)0.0737 (7)0.0615 (3)0.073 (3)
H1A0.75820.10170.04480.088*
C20.8185 (7)0.0001 (8)0.0505 (4)0.085 (4)
H2A0.80080.02090.02680.102*
C30.8710 (8)0.0426 (8)0.0745 (4)0.085 (4)
H3A0.88760.09230.06740.102*
C40.8983 (7)0.0092 (7)0.1097 (4)0.075 (3)
H4A0.93450.03600.12590.089*
C50.8703 (5)0.0650 (6)0.1202 (3)0.052 (2)
C60.8961 (6)0.1027 (6)0.1585 (3)0.052 (2)
C70.9533 (7)0.0694 (7)0.1835 (4)0.076 (3)
H7A0.97960.02360.17620.092*
C80.9718 (8)0.1034 (9)0.2193 (4)0.087 (4)
H8A1.00930.08070.23640.104*
C90.9328 (8)0.1720 (9)0.2288 (4)0.087 (4)
H9A0.94240.19660.25270.104*
C100.8784 (7)0.2033 (7)0.2013 (3)0.072 (3)
H10A0.85380.25070.20710.087*
C110.8851 (8)0.2876 (7)0.0529 (4)0.094 (5)
H11A0.87810.23680.04410.113*
C120.9327 (9)0.3389 (7)0.0301 (4)0.090 (4)
H12A0.95810.32240.00710.108*
C130.9402 (8)0.4149 (8)0.0432 (4)0.086 (4)
H13A0.97010.45090.02870.103*
C140.9025 (7)0.4370 (7)0.0784 (3)0.070 (3)
H14A0.90800.48740.08790.084*
C150.8567 (6)0.3820 (5)0.0989 (3)0.048 (2)
C160.8108 (6)0.4026 (6)0.1366 (3)0.051 (2)
C170.8208 (7)0.4743 (6)0.1554 (3)0.065 (3)
H17A0.85710.51090.14530.078*
C180.7770 (7)0.4909 (7)0.1891 (4)0.074 (3)
H18A0.78390.53830.20190.089*
C190.7234 (8)0.4368 (7)0.2034 (4)0.081 (4)
H19A0.69320.44690.22600.097*
C200.7145 (7)0.3662 (6)0.1838 (3)0.066 (3)
H20A0.67660.33020.19310.079*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.0442 (4)0.0397 (4)0.0470 (4)0.0004 (3)0.0005 (3)0.0027 (3)
V10.0443 (8)0.0353 (8)0.0452 (9)0.0023 (6)0.0019 (7)0.0032 (7)
V20.0442 (9)0.0494 (10)0.0419 (9)0.0087 (7)0.0041 (7)0.0050 (8)
N10.046 (4)0.050 (5)0.058 (5)0.013 (4)0.005 (4)0.010 (4)
N20.052 (5)0.066 (6)0.043 (5)0.005 (4)0.007 (4)0.002 (4)
N30.075 (6)0.052 (5)0.067 (6)0.006 (5)0.021 (5)0.002 (5)
N40.064 (5)0.041 (5)0.057 (5)0.006 (4)0.011 (4)0.003 (4)
O10.092 (8)0.068 (7)0.085 (8)0.040 (6)0.0000.000
O20.082 (5)0.054 (4)0.061 (5)0.000 (4)0.014 (4)0.007 (4)
O30.052 (4)0.079 (5)0.049 (4)0.007 (4)0.001 (3)0.003 (4)
O40.074 (5)0.053 (4)0.053 (4)0.020 (3)0.010 (3)0.001 (3)
O50.052 (4)0.091 (6)0.051 (4)0.007 (4)0.012 (3)0.011 (4)
O60.100 (6)0.062 (5)0.059 (5)0.022 (4)0.005 (4)0.017 (4)
O70.062 (6)0.072 (7)0.060 (6)0.034 (5)0.0000.000
C10.074 (7)0.074 (8)0.071 (8)0.021 (6)0.018 (6)0.026 (7)
C20.076 (8)0.083 (9)0.094 (10)0.022 (7)0.017 (7)0.043 (8)
C30.081 (8)0.077 (9)0.098 (10)0.020 (7)0.005 (8)0.035 (8)
C40.060 (7)0.067 (7)0.096 (9)0.030 (6)0.008 (6)0.013 (7)
C50.041 (5)0.048 (5)0.066 (7)0.001 (4)0.003 (5)0.002 (5)
C60.045 (5)0.056 (6)0.054 (6)0.011 (4)0.005 (4)0.006 (5)
C70.082 (8)0.063 (8)0.084 (9)0.008 (6)0.025 (7)0.008 (7)
C80.078 (8)0.120 (12)0.063 (8)0.006 (8)0.031 (7)0.019 (8)
C90.075 (8)0.124 (12)0.060 (8)0.021 (8)0.010 (6)0.007 (8)
C100.075 (7)0.079 (8)0.064 (7)0.001 (6)0.025 (6)0.015 (6)
C110.113 (10)0.073 (9)0.097 (10)0.018 (7)0.069 (9)0.015 (7)
C120.124 (11)0.067 (8)0.079 (9)0.008 (7)0.059 (8)0.005 (7)
C130.105 (10)0.073 (9)0.079 (9)0.012 (7)0.018 (7)0.021 (7)
C140.082 (8)0.059 (7)0.068 (8)0.018 (6)0.024 (6)0.002 (6)
C150.052 (5)0.039 (5)0.053 (6)0.001 (4)0.001 (4)0.007 (5)
C160.049 (6)0.047 (6)0.057 (6)0.005 (4)0.002 (5)0.013 (5)
C170.068 (7)0.055 (7)0.072 (8)0.022 (5)0.020 (6)0.007 (6)
C180.089 (8)0.055 (7)0.078 (9)0.012 (6)0.013 (7)0.009 (6)
C190.096 (9)0.067 (8)0.078 (9)0.013 (7)0.025 (7)0.018 (7)
C200.082 (7)0.050 (6)0.067 (7)0.014 (5)0.026 (6)0.021 (6)
Geometric parameters (Å, º) top
Cd1—O52.280 (6)C3—H3A0.930
Cd1—O32.313 (7)C4—C51.402 (14)
Cd1—N42.370 (8)C4—H4A0.930
Cd1—N32.373 (9)C5—C61.517 (13)
Cd1—N12.374 (7)C6—C71.389 (14)
Cd1—N22.401 (8)C7—C81.386 (16)
V1—O21.636 (7)C7—H7A0.930
V1—O31.676 (7)C8—C91.378 (18)
V1—O11.792 (3)C8—H8A0.930
V1—O41.813 (7)C9—C101.399 (16)
V2—O61.621 (7)C9—H9A0.930
V2—O51.655 (7)C10—H10A0.930
V2—O71.801 (3)C11—C121.408 (16)
V2—O41.832 (7)C11—H11A0.930
N1—C11.378 (12)C12—C131.387 (17)
N1—C51.382 (12)C12—H12A0.930
N2—C101.320 (13)C13—C141.399 (16)
N2—C61.338 (12)C13—H13A0.930
N3—C151.326 (12)C14—C151.392 (13)
N3—C111.348 (14)C14—H14A0.930
N4—C161.348 (12)C15—C161.528 (13)
N4—C201.356 (12)C16—C171.400 (13)
O1—V1i1.792 (3)C17—C181.381 (15)
O7—V2i1.801 (3)C17—H17A0.930
C1—C21.387 (15)C18—C191.365 (16)
C1—H1A0.930C18—H18A0.930
C2—C31.393 (17)C19—C201.393 (14)
C2—H2A0.930C19—H19A0.930
C3—C41.402 (16)C20—H20A0.930
O5—Cd1—O391.7 (3)C4—C3—H3A120.6
O5—Cd1—N4107.7 (3)C3—C4—C5119.1 (11)
O3—Cd1—N486.4 (3)C3—C4—H4A120.5
O5—Cd1—N391.9 (3)C5—C4—H4A120.5
O3—Cd1—N3156.4 (3)N1—C5—C4121.7 (10)
N4—Cd1—N370.3 (3)N1—C5—C6117.1 (8)
O5—Cd1—N188.7 (3)C4—C5—C6121.2 (9)
O3—Cd1—N1106.8 (3)N2—C6—C7120.9 (10)
N4—Cd1—N1158.9 (3)N2—C6—C5116.5 (8)
N3—Cd1—N196.7 (3)C7—C6—C5122.6 (9)
O5—Cd1—N2156.9 (3)C8—C7—C6120.9 (12)
O3—Cd1—N285.7 (3)C8—C7—H7A119.6
N4—Cd1—N295.1 (3)C6—C7—H7A119.6
N3—Cd1—N299.7 (3)C9—C8—C7117.9 (11)
N1—Cd1—N270.2 (3)C9—C8—H8A121.0
O2—V1—O3108.7 (4)C7—C8—H8A121.0
O2—V1—O1109.0 (4)C8—C9—C10117.6 (12)
O3—V1—O1111.6 (3)C8—C9—H9A121.2
O2—V1—O4108.7 (3)C10—C9—H9A121.2
O3—V1—O4107.4 (3)N2—C10—C9124.4 (12)
O1—V1—O4111.3 (4)N2—C10—H10A117.8
O6—V2—O5108.6 (4)C9—C10—H10A117.8
O6—V2—O7109.5 (4)N3—C11—C12122.7 (11)
O5—V2—O7111.2 (3)N3—C11—H11A118.7
O6—V2—O4109.1 (4)C12—C11—H11A118.7
O5—V2—O4108.1 (3)C13—C12—C11117.5 (11)
O7—V2—O4110.1 (4)C13—C12—H12A121.3
C1—N1—C5118.5 (8)C11—C12—H12A121.3
C1—N1—Cd1123.8 (6)C12—C13—C14119.6 (11)
C5—N1—Cd1117.4 (6)C12—C13—H13A120.2
C10—N2—C6118.2 (9)C14—C13—H13A120.2
C10—N2—Cd1123.3 (7)C15—C14—C13118.7 (11)
C6—N2—Cd1118.5 (6)C15—C14—H14A120.7
C15—N3—C11119.0 (9)C13—C14—H14A120.7
C15—N3—Cd1118.9 (7)N3—C15—C14122.5 (10)
C11—N3—Cd1121.7 (8)N3—C15—C16115.7 (8)
C16—N4—C20119.1 (9)C14—C15—C16121.8 (9)
C16—N4—Cd1117.1 (6)N4—C16—C17120.4 (9)
C20—N4—Cd1123.6 (7)N4—C16—C15117.4 (8)
V1—O1—V1i156.5 (8)C17—C16—C15122.2 (9)
V1—O3—Cd1131.3 (4)C18—C17—C16120.2 (10)
V1—O4—V2129.4 (4)C18—C17—H17A119.9
V2—O5—Cd1134.0 (4)C16—C17—H17A119.9
V2—O7—V2i148.5 (6)C19—C18—C17119.0 (11)
N1—C1—C2121.2 (11)C19—C18—H18A120.5
N1—C1—H1A119.4C17—C18—H18A120.5
C2—C1—H1A119.4C18—C19—C20119.4 (11)
C1—C2—C3120.6 (12)C18—C19—H19A120.3
C1—C2—H2A119.7C20—C19—H19A120.3
C3—C2—H2A119.7N4—C20—C19121.8 (10)
C2—C3—C4118.8 (11)N4—C20—H20A119.1
C2—C3—H3A120.6C19—C20—H20A119.1
Symmetry code: (i) x+1, y+1/2, z.
 

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