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The neutral complex trans-[VOCl2(H2O)2] co-crystallizes with di-2-pyridylamine hydro­chloride to provide the title compound, (C10H10N3)2[VCl2O(H2O)2]Cl2. The V-bound aqua ligands form two hydrogen bonds each. The amine functionality of the 2-(2-pyridylamino)pyridinium cation participates as a monovalent donor in the hydrogen bonding. In both instances, inter­stitial Cl- ions serve as hydrogen-bond acceptors. The three hydrogen bonds that are formed per anion give rise to one-dimensional chains along [100].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805016843/lh6432sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805016843/lh6432Isup2.hkl
Contains datablock I

CCDC reference: 277713

Key indicators

  • Single-crystal X-ray study
  • T = 303 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.034
  • wR factor = 0.097
  • Data-to-parameter ratio = 15.3

checkCIF/PLATON results

No syntax errors found



Alert level C CRYSC01_ALERT_1_C The word below has not been recognised as a standard identifier. turquoise CRYSC01_ALERT_1_C No recognised colour has been given for crystal colour. RADNW01_ALERT_1_C The radiation wavelength lies outside the expected range for the supplied radiation type. Expected range 0.71065-0.71075 Wavelength given = 0.71093 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT230_ALERT_2_C Hirshfeld Test Diff for N5 - C16 .. 5.15 su PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for V1 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.25 PLAT353_ALERT_3_C Long N-H Bond (0.87A) N3 - H3N ... 1.07 Ang. PLAT353_ALERT_3_C Long N-H Bond (0.87A) N6 - H6N ... 1.07 Ang. PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.838(10) ...... 3.00 su-Rat O2 -H2B 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.838(10) ...... 3.00 su-Rat O2 -H2B 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 2.19(3), Rep 2.189(12) ...... 2.50 su-Rat H2A -CL3 1.555 2.566 PLAT736_ALERT_1_C H...A Calc 2.21(3), Rep 2.203(13) ...... 2.31 su-Rat H2B -CL4 1.555 2.566
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 13 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 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: CAD-4 Diffractometer Control Software (Enraf–Nonius, 1993); cell refinement: CAD-4 Diffractometer Control Software; data reduction: CAD-4 Diffractometer Control Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON2003 (Spek, 1990, 2003) and ORTEP-3 (Farrugia, 1997, 2005); software used to prepare material for publication: SHELXL97.

trans-Diaquadichlorooxovanadium(IV) bis[2-(2-pyridylamino)pyridinium] dichloride top
Crystal data top
(C10H10N3)2[VCl2O(H2O)2]Cl2Z = 2
Mr = 589.19F(000) = 602
Triclinic, P1Dx = 1.519 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71093 Å
a = 7.838 (2) ÅCell parameters from 25 reflections
b = 9.609 (1) Åθ = 3.2–10.1°
c = 17.739 (3) ŵ = 0.83 mm1
α = 86.68 (1)°T = 303 K
β = 86.10 (2)°Prism, turquoise
γ = 75.32 (1)°0.25 × 0.15 × 0.10 mm
V = 1288.3 (4) Å3
Data collection top
Enraf–Nonius CAD-4
diffractometer
3771 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.024
Graphite monochromatorθmax = 26.0°, θmin = 1.2°
ω/2θ scansh = 93
Absorption correction: ψ scan
(North et al., 1968)
k = 1111
Tmin = 0.735, Tmax = 0.918l = 2121
6971 measured reflections3 standard reflections every 120 min
5048 independent reflections intensity decay: 0.1%
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)] = 0.034Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.097H atoms treated by a mixture of independent and constrained refinement
S = 1.01 w = 1/[σ2(Fo2) + (0.054P)2 + 0.4055P]
where P = (Fo2 + 2Fc2)/3
5048 reflections(Δ/σ)max = 0.001
331 parametersΔρmax = 0.50 e Å3
6 restraintsΔρmin = 0.39 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
C10.2356 (3)0.5770 (3)0.00722 (14)0.0451 (6)
C20.2178 (4)0.7260 (3)0.01530 (16)0.0554 (7)
H20.24410.77610.02390.067*
C30.1615 (4)0.7960 (3)0.08136 (17)0.0626 (8)
H30.15040.89460.08750.075*
C40.1202 (5)0.7218 (4)0.13987 (17)0.0633 (8)
H40.08050.76970.18490.076*
C50.1394 (4)0.5787 (3)0.12967 (16)0.0566 (7)
H50.11370.52750.16850.068*
C60.3150 (3)0.3568 (3)0.07531 (15)0.0470 (6)
C70.3717 (4)0.3015 (4)0.14605 (17)0.0596 (7)
H70.39320.36080.18200.072*
C80.3948 (5)0.1575 (4)0.1610 (2)0.0723 (9)
H80.43260.11690.20780.087*
C90.3622 (5)0.0725 (4)0.1070 (2)0.0806 (10)
H90.37790.02600.11640.097*
C100.3065 (5)0.1355 (4)0.0397 (2)0.0737 (9)
H100.28510.07720.00320.088*
C110.3392 (3)0.4737 (3)0.44131 (14)0.0393 (5)
C120.4408 (3)0.4686 (3)0.37369 (15)0.0481 (6)
H120.45280.55310.34810.058*
C130.5229 (4)0.3377 (3)0.34528 (15)0.0497 (6)
H130.59290.33320.30060.060*
C140.5027 (3)0.2115 (3)0.38255 (15)0.0480 (6)
H140.55760.12240.36310.058*
C150.4014 (3)0.2208 (3)0.44783 (14)0.0432 (6)
H150.38650.13690.47320.052*
C160.1544 (3)0.6259 (3)0.53953 (13)0.0400 (5)
C170.0865 (3)0.7673 (3)0.56181 (15)0.0450 (6)
H170.10880.84490.53250.054*
C180.0131 (4)0.7874 (3)0.62793 (16)0.0519 (7)
H180.06100.88010.64440.062*
C190.0432 (4)0.6706 (3)0.67057 (16)0.0532 (7)
H190.10950.68320.71630.064*
C200.0263 (4)0.5357 (3)0.64431 (15)0.0503 (6)
H200.00400.45710.67270.060*
N10.2911 (3)0.5019 (3)0.05707 (13)0.0534 (6)
H1N0.320 (4)0.551 (3)0.0920 (18)0.064*
N20.2807 (3)0.2758 (3)0.02265 (13)0.0567 (6)
N30.1948 (3)0.5081 (3)0.06445 (12)0.0473 (5)
H3N0.225 (4)0.398 (3)0.0447 (16)0.057*
N40.2567 (3)0.6006 (2)0.47345 (13)0.0475 (5)
H4N0.272 (4)0.675 (3)0.4466 (16)0.057*
N50.1246 (3)0.5121 (2)0.57994 (12)0.0461 (5)
N60.3214 (3)0.3497 (2)0.47687 (12)0.0400 (4)
H6N0.245 (4)0.380 (3)0.5282 (15)0.048*
O10.2079 (3)0.0399 (2)0.75522 (11)0.0624 (5)
O20.1269 (2)0.1593 (3)0.73546 (12)0.0730 (7)
H2A0.180 (4)0.150 (4)0.6974 (11)0.088*
H2B0.203 (3)0.203 (4)0.7670 (13)0.088*
O30.3382 (3)0.2104 (3)0.72630 (11)0.0621 (6)
H3A0.417 (3)0.189 (4)0.6911 (11)0.075*
H3B0.387 (3)0.233 (3)0.7626 (11)0.075*
V10.13210 (5)0.12565 (4)0.73736 (2)0.03288 (11)
Cl10.07551 (10)0.23032 (9)0.85385 (4)0.0619 (2)
Cl20.13293 (8)0.14329 (7)0.60732 (3)0.04341 (15)
Cl30.35957 (8)0.86934 (6)0.38838 (3)0.04221 (15)
Cl40.44189 (9)0.67355 (8)0.17119 (4)0.0577 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0397 (13)0.0554 (15)0.0407 (13)0.0146 (12)0.0055 (11)0.0041 (11)
C20.0620 (18)0.0618 (17)0.0504 (15)0.0298 (14)0.0011 (13)0.0082 (13)
C30.077 (2)0.0527 (17)0.0634 (18)0.0289 (16)0.0009 (16)0.0040 (14)
C40.074 (2)0.071 (2)0.0503 (16)0.0281 (17)0.0094 (15)0.0096 (14)
C50.0658 (19)0.0634 (18)0.0453 (15)0.0230 (15)0.0086 (13)0.0025 (13)
C60.0405 (14)0.0523 (15)0.0475 (14)0.0108 (12)0.0006 (11)0.0025 (11)
C70.0583 (18)0.068 (2)0.0537 (16)0.0151 (15)0.0144 (14)0.0028 (14)
C80.070 (2)0.073 (2)0.066 (2)0.0035 (18)0.0172 (17)0.0112 (17)
C90.091 (3)0.0523 (19)0.091 (3)0.0032 (18)0.016 (2)0.0055 (18)
C100.092 (3)0.0536 (19)0.074 (2)0.0105 (17)0.0137 (19)0.0147 (16)
C110.0346 (12)0.0390 (13)0.0458 (13)0.0085 (10)0.0112 (10)0.0075 (10)
C120.0458 (14)0.0466 (15)0.0547 (15)0.0161 (12)0.0092 (12)0.0017 (12)
C130.0410 (14)0.0620 (17)0.0464 (14)0.0127 (13)0.0006 (11)0.0081 (12)
C140.0418 (14)0.0466 (15)0.0527 (15)0.0030 (11)0.0031 (12)0.0147 (12)
C150.0444 (14)0.0359 (12)0.0484 (14)0.0058 (11)0.0088 (11)0.0068 (10)
C160.0371 (12)0.0401 (13)0.0437 (13)0.0071 (10)0.0105 (10)0.0113 (10)
C170.0444 (14)0.0332 (12)0.0580 (15)0.0066 (11)0.0123 (12)0.0094 (11)
C180.0473 (15)0.0424 (14)0.0637 (17)0.0004 (12)0.0130 (13)0.0218 (12)
C190.0474 (15)0.0596 (17)0.0497 (15)0.0044 (13)0.0051 (12)0.0162 (13)
C200.0573 (17)0.0453 (15)0.0470 (14)0.0095 (13)0.0046 (12)0.0027 (11)
N10.0642 (15)0.0598 (15)0.0426 (12)0.0232 (12)0.0099 (11)0.0133 (10)
N20.0661 (15)0.0523 (14)0.0506 (13)0.0098 (12)0.0079 (11)0.0099 (10)
N30.0506 (13)0.0516 (13)0.0412 (11)0.0141 (10)0.0019 (9)0.0085 (9)
N40.0559 (14)0.0344 (11)0.0534 (13)0.0146 (10)0.0011 (11)0.0003 (9)
N50.0522 (13)0.0360 (11)0.0493 (12)0.0089 (10)0.0048 (10)0.0042 (9)
N60.0408 (11)0.0360 (10)0.0424 (11)0.0062 (9)0.0055 (9)0.0064 (8)
O10.0846 (15)0.0427 (11)0.0543 (11)0.0075 (10)0.0024 (10)0.0043 (8)
O20.0316 (10)0.137 (2)0.0537 (12)0.0191 (12)0.0028 (8)0.0461 (13)
O30.0466 (11)0.1086 (17)0.0476 (11)0.0466 (12)0.0054 (9)0.0268 (11)
V10.0316 (2)0.0362 (2)0.0333 (2)0.01211 (16)0.00178 (15)0.00509 (15)
Cl10.0529 (4)0.0962 (6)0.0468 (4)0.0334 (4)0.0070 (3)0.0337 (4)
Cl20.0460 (3)0.0529 (4)0.0358 (3)0.0202 (3)0.0044 (2)0.0016 (2)
Cl30.0377 (3)0.0454 (3)0.0480 (3)0.0176 (3)0.0031 (2)0.0057 (2)
Cl40.0396 (3)0.0751 (5)0.0636 (4)0.0173 (3)0.0019 (3)0.0354 (4)
Geometric parameters (Å, º) top
C1—N31.342 (3)C14—C151.353 (4)
C1—N11.350 (3)C14—H140.9300
C1—C21.403 (4)C15—N61.352 (3)
C2—C31.360 (4)C15—H150.9300
C2—H20.9300C16—N51.334 (3)
C3—C41.393 (4)C16—N41.372 (3)
C3—H30.9300C16—C171.398 (3)
C4—C51.348 (4)C17—C181.359 (4)
C4—H40.9300C17—H170.9300
C5—N31.347 (3)C18—C191.378 (4)
C5—H50.9300C18—H180.9300
C6—N21.332 (3)C19—C201.368 (4)
C6—N11.381 (4)C19—H190.9300
C6—C71.391 (4)C20—N51.331 (3)
C7—C81.362 (5)C20—H200.9300
C7—H70.9300N1—H1N0.87 (3)
C8—C91.371 (5)N3—H3N1.07 (3)
C8—H80.9300N4—H4N0.86 (3)
C9—C101.355 (5)N6—H6N1.07 (3)
C9—H90.9300O1—V11.5719 (19)
C10—N21.332 (4)O2—V11.9753 (19)
C10—H100.9300O2—H2A0.837 (10)
C11—N61.350 (3)O2—H2B0.838 (10)
C11—N41.364 (3)O3—V11.9791 (18)
C11—C121.390 (4)O3—H3A0.845 (10)
C12—C131.367 (4)O3—H3B0.839 (10)
C12—H120.9300V1—Cl22.3030 (8)
C13—C141.386 (4)V1—Cl12.3169 (8)
C13—H130.9300
N3—C1—N1119.4 (2)N5—C16—N4117.6 (2)
N3—C1—C2119.1 (2)N5—C16—C17122.9 (2)
N1—C1—C2121.5 (2)N4—C16—C17119.5 (2)
C3—C2—C1118.9 (3)C18—C17—C16117.6 (3)
C3—C2—H2120.6C18—C17—H17121.2
C1—C2—H2120.6C16—C17—H17121.2
C2—C3—C4120.8 (3)C17—C18—C19120.1 (2)
C2—C3—H3119.6C17—C18—H18120.0
C4—C3—H3119.6C19—C18—H18120.0
C5—C4—C3118.3 (3)C20—C19—C18118.7 (3)
C5—C4—H4120.8C20—C19—H19120.6
C3—C4—H4120.8C18—C19—H19120.6
N3—C5—C4121.5 (3)N5—C20—C19122.8 (3)
N3—C5—H5119.3N5—C20—H20118.6
C4—C5—H5119.3C19—C20—H20118.6
N2—C6—N1116.9 (2)C1—N1—C6129.6 (2)
N2—C6—C7122.9 (3)C1—N1—H1N116 (2)
N1—C6—C7120.1 (3)C6—N1—H1N114 (2)
C8—C7—C6117.9 (3)C10—N2—C6117.0 (3)
C8—C7—H7121.1C1—N3—C5121.4 (2)
C6—C7—H7121.1C1—N3—H3N103.7 (15)
C7—C8—C9119.8 (3)C5—N3—H3N134.8 (15)
C7—C8—H8120.1C11—N4—C16130.0 (2)
C9—C8—H8120.1C11—N4—H4N113 (2)
C10—C9—C8118.5 (3)C16—N4—H4N117 (2)
C10—C9—H9120.8C20—N5—C16117.9 (2)
C8—C9—H9120.8C11—N6—C15121.0 (2)
N2—C10—C9123.9 (3)C11—N6—H6N105.8 (14)
N2—C10—H10118.1C15—N6—H6N133.1 (14)
C9—C10—H10118.1V1—O2—H2A124 (2)
N6—C11—N4118.5 (2)V1—O2—H2B127 (2)
N6—C11—C12119.4 (2)H2A—O2—H2B107.3 (16)
N4—C11—C12122.1 (2)V1—O3—H3A123 (2)
C13—C12—C11119.2 (3)V1—O3—H3B124 (2)
C13—C12—H12120.4H3A—O3—H3B106.1 (15)
C11—C12—H12120.4O1—V1—O2106.87 (12)
C12—C13—C14120.6 (3)O1—V1—O3106.15 (12)
C12—C13—H13119.7O2—V1—O3146.98 (12)
C14—C13—H13119.7O1—V1—Cl2103.59 (8)
C15—C14—C13118.6 (2)O2—V1—Cl286.12 (7)
C15—C14—H14120.7O3—V1—Cl286.13 (6)
C13—C14—H14120.7O1—V1—Cl1105.55 (8)
N6—C15—C14121.3 (2)O2—V1—Cl185.55 (6)
N6—C15—H15119.4O3—V1—Cl185.80 (6)
C14—C15—H15119.4Cl2—V1—Cl1150.85 (3)
N3—C1—C2—C30.8 (4)N3—C1—N1—C60.2 (4)
N1—C1—C2—C3180.0 (3)C2—C1—N1—C6179.4 (3)
C1—C2—C3—C40.7 (5)N2—C6—N1—C10.6 (4)
C2—C3—C4—C50.7 (5)C7—C6—N1—C1179.1 (3)
C3—C4—C5—N30.8 (5)C9—C10—N2—C61.1 (5)
N2—C6—C7—C80.9 (5)N1—C6—N2—C10178.9 (3)
N1—C6—C7—C8179.4 (3)C7—C6—N2—C101.4 (4)
C6—C7—C8—C90.0 (5)N1—C1—N3—C5179.8 (3)
C7—C8—C9—C100.3 (6)C2—C1—N3—C50.9 (4)
C8—C9—C10—N20.3 (6)C4—C5—N3—C10.9 (4)
N6—C11—C12—C131.0 (4)N6—C11—N4—C160.7 (4)
N4—C11—C12—C13178.7 (2)C12—C11—N4—C16179.0 (3)
C11—C12—C13—C141.2 (4)N5—C16—N4—C111.4 (4)
C12—C13—C14—C150.6 (4)C17—C16—N4—C11178.5 (2)
C13—C14—C15—N60.3 (4)C19—C20—N5—C160.6 (4)
N5—C16—C17—C180.3 (4)N4—C16—N5—C20179.6 (2)
N4—C16—C17—C18179.5 (2)C17—C16—N5—C200.2 (4)
C16—C17—C18—C190.4 (4)N4—C11—N6—C15179.5 (2)
C17—C18—C19—C201.1 (4)C12—C11—N6—C150.2 (3)
C18—C19—C20—N51.2 (4)C14—C15—N6—C110.4 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1N···Cl40.87 (3)2.29 (3)3.149 (2)170 (3)
N3—H3N···N21.07 (3)1.62 (3)2.608 (3)150 (2)
N4—H4N···Cl30.86 (3)2.32 (3)3.168 (2)169 (3)
N6—H6N···N51.07 (3)1.66 (3)2.624 (3)148 (2)
O2—H2A···Cl3i0.84 (1)2.19 (1)3.016 (2)170 (3)
O2—H2B···Cl4i0.84 (1)2.20 (1)3.026 (2)167 (3)
O3—H3B···Cl4ii0.84 (1)2.22 (1)3.0259 (19)162 (3)
O3—H3B···Cl4ii0.84 (1)2.22 (1)3.0259 (19)162 (3)
Symmetry codes: (i) x, y+1, z+1; (ii) x+1, y+1, z+1.
 

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