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In the title complex, [V(C2O4)O(C12H8N2)(H2O)], a 1,10-phenanthroline mol­ecule and an oxalate dianion chelate to the VIV atom, the distorted octahedral coordination of which is completed by a water mol­ecule and an oxo O atom. The complex mol­ecules are linked across a centre of inversion to form a hydrogen-bonded dimer, and these dimers are linked by another hydrogen bond into a linear chain.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804024432/hb6202sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804024432/hb6202Isup2.hkl
Contains datablock I

CCDC reference: 255408

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.043
  • wR factor = 0.125
  • Data-to-parameter ratio = 14.4

checkCIF/PLATON results

No syntax errors found



Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.804 0.943 Tmin' and Tmax expected: 0.899 0.942 RR' = 0.894 Please check that your absorption correction is appropriate. PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.89 PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C13 - C14 ... 1.56 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
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: C14 H10 N2 O6 V1 Atom count from _chemical_formula_moiety:C14 H10 N2 O5 V1
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 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 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 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, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Aqua(oxalato-κ2O,O')oxo(1,10-phenanthroline-κ2N,N')vanadium(IV) top
Crystal data top
[V(C2O4)O(C12H8N2)(H2O)]Z = 2
Mr = 353.18F(000) = 358
Triclinic, P1Dx = 1.682 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.6328 (7) ÅCell parameters from 1906 reflections
b = 9.7800 (9) Åθ = 2.8–24.3°
c = 9.8622 (9) ŵ = 0.75 mm1
α = 89.351 (1)°T = 295 K
β = 73.954 (1)°Prism, green
γ = 80.565 (1)°0.14 × 0.10 × 0.08 mm
V = 697.5 (1) Å3
Data collection top
Bruker APEX CCD area-detector
diffractometer
3105 independent reflections
Radiation source: fine-focus sealed tube2406 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
φ and ω scansθmax = 27.5°, θmin = 2.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 99
Tmin = 0.804, Tmax = 0.943k = 1212
7736 measured reflectionsl = 1212
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)] = 0.043Hydrogen site location: difmap (O-H) and geom (C-H)
wR(F2) = 0.125H atoms treated by a mixture of independent and constrained refinement
S = 1.05 w = 1/[σ2(Fo2) + (0.0717P)2 + 0.0065P]
where P = (Fo2 + 2Fc2)/3
3105 reflections(Δ/σ)max = 0.001
216 parametersΔρmax = 0.39 e Å3
3 restraintsΔρmin = 0.26 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
V10.51066 (6)0.39347 (4)0.73480 (5)0.0255 (2)
O10.7137 (2)0.3988 (2)0.5586 (2)0.0322 (4)
O21.0198 (3)0.3471 (2)0.4718 (2)0.0477 (6)
O30.7275 (2)0.3323 (2)0.81050 (19)0.0321 (4)
O41.0336 (3)0.2842 (2)0.7449 (2)0.0497 (6)
O50.4474 (3)0.5495 (2)0.7930 (2)0.0491 (6)
O1W0.3337 (3)0.3910 (2)0.6140 (2)0.0388 (5)
N10.3270 (3)0.3145 (2)0.9085 (2)0.0253 (5)
N20.5494 (3)0.1565 (2)0.6903 (2)0.0288 (5)
C10.3225 (4)0.1763 (3)0.9120 (3)0.0279 (6)
C20.2165 (4)0.3934 (3)1.0170 (3)0.0371 (7)
C30.0970 (4)0.3415 (4)1.1311 (3)0.0477 (8)
C40.0916 (4)0.2049 (4)1.1346 (3)0.0481 (8)
C50.2091 (4)0.1149 (3)1.0245 (3)0.0372 (7)
C60.2178 (5)0.0323 (3)1.0200 (4)0.0481 (8)
C70.3329 (5)0.1124 (3)0.9121 (4)0.0490 (9)
C80.4492 (4)0.0541 (3)0.7950 (3)0.0374 (7)
C90.5747 (5)0.1312 (3)0.6787 (4)0.0493 (9)
C100.6794 (5)0.0643 (3)0.5729 (4)0.0473 (8)
C110.6637 (4)0.0778 (3)0.5825 (3)0.0390 (7)
C120.4450 (4)0.0903 (3)0.7958 (3)0.0282 (6)
C130.8798 (4)0.3583 (3)0.5677 (3)0.0295 (6)
C140.8864 (4)0.3203 (3)0.7209 (3)0.0305 (6)
H1W10.329 (4)0.457 (2)0.560 (3)0.05 (1)*
H1W20.229 (2)0.364 (3)0.638 (3)0.05 (1)*
H20.21920.48811.01660.045*
H30.02120.40091.20450.057*
H40.01020.16971.20990.058*
H60.14160.07341.09380.058*
H70.33710.20800.91370.059*
H90.58600.22730.67420.059*
H100.76120.11410.49470.057*
H110.73730.12130.50930.047*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0250 (3)0.0205 (2)0.0307 (3)0.0059 (2)0.0063 (2)0.0053 (2)
O10.027 (1)0.039 (1)0.032 (1)0.006 (1)0.010 (1)0.015 (1)
O20.032 (1)0.064 (2)0.039 (1)0.001 (1)0.001 (1)0.005 (1)
O30.030 (1)0.041 (1)0.028 (1)0.014 (1)0.008 (1)0.008 (1)
O40.032 (1)0.074 (2)0.052 (1)0.017 (1)0.022 (1)0.029 (1)
O50.053 (1)0.024 (1)0.062 (2)0.010 (1)0.001 (1)0.001 (1)
O1W0.029 (1)0.044 (1)0.049 (1)0.013 (1)0.018 (1)0.022 (1)
N10.027 (1)0.021 (1)0.029 (1)0.005 (1)0.009 (1)0.003 (1)
N20.028 (1)0.025 (1)0.034 (1)0.003 (1)0.011 (1)0.001 (1)
C10.031 (1)0.028 (1)0.032 (1)0.011 (1)0.016 (1)0.008 (1)
C20.042 (2)0.034 (2)0.034 (2)0.010 (1)0.007 (1)0.003 (1)
C30.049 (2)0.055 (2)0.032 (2)0.010 (2)0.002 (1)0.003 (1)
C40.050 (2)0.064 (2)0.033 (2)0.024 (2)0.008 (2)0.017 (2)
C50.039 (2)0.042 (2)0.040 (2)0.019 (1)0.018 (1)0.016 (1)
C60.054 (2)0.042 (2)0.060 (2)0.024 (2)0.027 (2)0.030 (2)
C70.060 (2)0.030 (2)0.071 (2)0.023 (2)0.033 (2)0.019 (2)
C80.042 (2)0.024 (1)0.0563 (19)0.006 (1)0.030 (2)0.005 (1)
C90.061 (2)0.025 (2)0.070 (2)0.004 (2)0.033 (2)0.007 (2)
C100.049 (2)0.033 (2)0.057 (2)0.008 (1)0.018 (2)0.016 (2)
C110.036 (2)0.038 (2)0.041 (2)0.004 (1)0.009 (1)0.005 (1)
C120.031 (1)0.023 (1)0.037 (2)0.009 (1)0.018 (1)0.006 (1)
C130.032 (1)0.025 (1)0.033 (2)0.006 (1)0.010 (1)0.005 (1)
C140.032 (2)0.026 (1)0.039 (2)0.011 (1)0.015 (1)0.009 (1)
Geometric parameters (Å, º) top
V1—O11.990 (2)C5—C61.431 (4)
V1—O32.001 (2)C6—C71.340 (5)
V1—O51.586 (2)C7—C81.426 (5)
V1—O1W2.036 (2)C8—C91.406 (5)
V1—N12.120 (2)C8—C121.407 (4)
V1—N22.319 (2)C9—C101.361 (5)
O1—C131.292 (3)C10—C111.377 (4)
O2—C131.206 (3)C13—C141.564 (4)
O3—C141.277 (3)O1W—H1W10.84 (1)
O4—C141.207 (3)O1W—H1W20.86 (1)
N1—C21.326 (3)C2—H20.93
N1—C11.357 (3)C3—H30.93
N2—C111.330 (3)C4—H40.93
N2—C121.354 (3)C6—H60.93
C1—C51.402 (4)C7—H70.93
C1—C121.437 (4)C9—H90.93
C2—C31.388 (4)C10—H100.93
C3—C41.343 (4)C11—H110.93
C4—C51.409 (4)
O1—V1—O380.8 (1)C9—C8—C12116.6 (3)
O1—V1—O5105.3 (1)C9—C8—C7124.6 (3)
O1—V1—O1W88.7 (1)C12—C8—C7118.7 (3)
O1—V1—N1160.4 (1)C10—C9—C8119.5 (3)
O1—V1—N287.2 (1)C9—C10—C11119.6 (3)
O3—V1—O5101.8 (1)N2—C11—C10123.8 (3)
O3—V1—O1W158.9 (1)N2—C12—C8123.6 (3)
O3—V1—N192.4 (1)N2—C12—C1116.3 (2)
O3—V1—N280.9 (1)C8—C12—C1120.1 (3)
O5—V1—O1W98.5 (1)O2—C13—O1126.2 (3)
O5—V1—N194.0 (1)O2—C13—C14120.8 (2)
O5—V1—N2167.5 (1)O1—C13—C14113.0 (2)
O1W—V1—N191.6 (1)O4—C14—O3126.2 (3)
O1W—V1—N280.4 (1)O4—C14—C13119.8 (2)
N1—V1—N273.6 (1)O3—C14—C13113.9 (2)
C13—O1—V1116.2 (2)V1—O1W—H1W1115 (2)
C14—O3—V1116.0 (2)V1—O1W—H1W2127 (2)
C2—N1—C1117.5 (2)H1W1—O1W—H1W2109 (2)
C2—N1—V1123.2 (2)N1—C2—H2118.4
C1—N1—V1119.3 (2)C3—C2—H2118.4
C11—N2—C12116.8 (2)C4—C3—H3120.2
C11—N2—V1129.9 (2)C2—C3—H3120.2
C12—N2—V1113.2 (2)C3—C4—H4120.0
N1—C1—C5123.1 (3)C5—C4—H4120.0
N1—C1—C12117.5 (2)C7—C6—H6119.2
C5—C1—C12119.4 (2)C5—C6—H6119.2
N1—C2—C3123.2 (3)C6—C7—H7119.4
C4—C3—C2119.6 (3)C8—C7—H7119.4
C3—C4—C5120.0 (3)C10—C9—H9120.2
C1—C5—C4116.6 (3)C8—C9—H9120.2
C1—C5—C6118.9 (3)C9—C10—H10120.2
C4—C5—C6124.5 (3)C11—C10—H10120.2
C7—C6—C5121.6 (3)N2—C11—H11118.1
C6—C7—C8121.3 (3)C10—C11—H11118.1
O5—V1—O1—C13102.7 (2)N1—C1—C5—C42.3 (4)
O3—V1—O1—C132.85 (18)C12—C1—C5—C4179.7 (2)
O1W—V1—O1—C13158.81 (19)N1—C1—C5—C6178.4 (2)
N1—V1—O1—C1367.8 (3)C12—C1—C5—C60.4 (4)
N2—V1—O1—C1378.38 (19)C3—C4—C5—C12.5 (4)
O5—V1—O3—C14105.7 (2)C3—C4—C5—C6178.2 (3)
O1—V1—O3—C141.88 (18)C1—C5—C6—C70.8 (4)
O1W—V1—O3—C1459.1 (3)C4—C5—C6—C7179.9 (3)
N1—V1—O3—C14159.68 (19)C5—C6—C7—C81.5 (5)
N2—V1—O3—C1486.70 (19)C6—C7—C8—C9179.3 (3)
O5—V1—N1—C21.8 (2)C6—C7—C8—C121.7 (4)
O1—V1—N1—C2169.0 (2)C12—C8—C9—C102.0 (4)
O3—V1—N1—C2100.2 (2)C7—C8—C9—C10179.7 (3)
O1W—V1—N1—C2100.5 (2)C8—C9—C10—C111.2 (5)
N2—V1—N1—C2180.0 (2)C12—N2—C11—C100.5 (4)
O5—V1—N1—C1179.30 (19)V1—N2—C11—C10176.3 (2)
O1—V1—N1—C19.9 (3)C9—C10—C11—N20.5 (5)
O3—V1—N1—C178.65 (18)C11—N2—C12—C81.4 (4)
O1W—V1—N1—C180.63 (19)V1—N2—C12—C8177.9 (2)
N2—V1—N1—C11.15 (17)C11—N2—C12—C1179.8 (2)
O5—V1—N2—C11173.2 (5)V1—N2—C12—C13.2 (3)
O1—V1—N2—C112.0 (2)C9—C8—C12—N22.2 (4)
O3—V1—N2—C1183.1 (2)C7—C8—C12—N2180.0 (3)
O1W—V1—N2—C1187.1 (2)C9—C8—C12—C1179.0 (3)
N1—V1—N2—C11178.3 (2)C7—C8—C12—C11.2 (4)
O5—V1—N2—C1210.9 (6)N1—C1—C12—N22.4 (3)
O1—V1—N2—C12173.96 (18)C5—C1—C12—N2179.5 (2)
O3—V1—N2—C1292.82 (18)N1—C1—C12—C8178.7 (2)
O1W—V1—N2—C1296.93 (18)C5—C1—C12—C80.6 (4)
N1—V1—N2—C122.36 (17)V1—O1—C13—O2175.9 (2)
C2—N1—C1—C50.7 (4)V1—O1—C13—C143.1 (3)
V1—N1—C1—C5178.22 (19)V1—O3—C14—O4179.6 (2)
C2—N1—C1—C12178.8 (2)V1—O3—C14—C130.8 (3)
V1—N1—C1—C120.2 (3)O2—C13—C14—O42.9 (4)
C1—N1—C2—C30.8 (4)O1—C13—C14—O4178.1 (3)
V1—N1—C2—C3179.7 (2)O2—C13—C14—O3177.5 (3)
N1—C2—C3—C40.5 (5)O1—C13—C14—O31.6 (3)
C2—C3—C4—C51.2 (5)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O1i0.84 (1)1.86 (1)2.697 (3)173 (3)
O1W—H1W2···O4ii0.86 (1)1.85 (1)2.671 (3)160 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x1, y, z.
 

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