Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807054529/at2459sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807054529/at2459Isup2.hkl |
CCDC reference: 1176495
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (C-C) = 0.007 Å
- R factor = 0.051
- wR factor = 0.177
- Data-to-parameter ratio = 16.3
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.95 PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) V1 - N1 .. 11.19 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) V1 - N2 .. 10.29 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) V1 - N3 .. 10.60 su
Alert level C PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.29 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N3 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for V1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C11 PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 7
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for V1 (3) 2.56
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 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 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For a related structure, see: Liu & Zhu (2007). For bond-length data, see: Allen et al. (1987).
Crystals of the title compound were synthesized using hydrothermal method in a Teflon-lined Parr bomb (23 ml), which was then sealed. Lanthanum (III) nitrate hexahydrate (432.4 mg, 1 mmol), vanadium dichloride (243.6 mg, 2 mmol), potassium thiocyanate (194.2 mg, 2 mmol), pyridine (6 ml), and distilled water (10 g) were placed into the bomb and sealed. The bomb was heated under autogenous pressure for 7 d at 453 K and allowed to cool at room temperature for 24 h. Upon opening the bomb, a clear colourless solution was decanted from small colourless crystals. These crystals were washed with distilled water followed by ethanol, and allowed to air-dry at room temperature.
H atoms were positioned geometrically, with C—H = 0.93 Å for aromatic H and constrained to ride on their parent atoms, with Uiso(H) = 1.2Ueq(C).
Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1996); software used to prepare material for publication: SHELXTL (Siemens, 1996).
[V(NCS)2(C5H5N)4] | F(000) = 996 |
Mr = 483.50 | Dx = 1.377 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 4483 reflections |
a = 12.5011 (13) Å | θ = 2.5–27.9° |
b = 13.003 (3) Å | µ = 0.63 mm−1 |
c = 14.999 (3) Å | T = 273 K |
β = 106.981 (5)° | Block, colourless |
V = 2331.8 (8) Å3 | 0.31 × 0.29 × 0.16 mm |
Z = 4 |
Bruker APEX-II area-detector diffractometer | 2332 independent reflections |
Radiation source: fine-focus sealed tube | 1933 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.020 |
ϕ and ω scans | θmax = 26.6°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −15→15 |
Tmin = 0.827, Tmax = 0.904 | k = −16→16 |
7623 measured reflections | l = −18→18 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.051 | H-atom parameters constrained |
wR(F2) = 0.178 | w = 1/[σ2(Fo2) + (0.1448P)2 + 1.8328P] where P = (Fo2 + 2Fc2)/3 |
S = 1.04 | (Δ/σ)max < 0.001 |
2332 reflections | Δρmax = 1.34 e Å−3 |
143 parameters | Δρmin = −0.58 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.018 (3) |
[V(NCS)2(C5H5N)4] | V = 2331.8 (8) Å3 |
Mr = 483.50 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 12.5011 (13) Å | µ = 0.63 mm−1 |
b = 13.003 (3) Å | T = 273 K |
c = 14.999 (3) Å | 0.31 × 0.29 × 0.16 mm |
β = 106.981 (5)° |
Bruker APEX-II area-detector diffractometer | 2332 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 1933 reflections with I > 2σ(I) |
Tmin = 0.827, Tmax = 0.904 | Rint = 0.020 |
7623 measured reflections |
R[F2 > 2σ(F2)] = 0.051 | 0 restraints |
wR(F2) = 0.178 | H-atom parameters constrained |
S = 1.04 | Δρmax = 1.34 e Å−3 |
2332 reflections | Δρmin = −0.58 e Å−3 |
143 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. |
x | y | z | Uiso*/Ueq | ||
V1 | 0.7500 | 0.7500 | 0.5000 | 0.0357 (3) | |
S1 | 1.07294 (10) | 0.64360 (9) | 0.41903 (9) | 0.0802 (4) | |
N1 | 0.7867 (2) | 0.6901 (2) | 0.6395 (2) | 0.0585 (7) | |
N2 | 0.6400 (2) | 0.6220 (2) | 0.4417 (2) | 0.0585 (7) | |
N3 | 0.8866 (2) | 0.6723 (3) | 0.4824 (2) | 0.0632 (8) | |
C1 | 0.8412 (3) | 0.6005 (3) | 0.6643 (3) | 0.0694 (10) | |
H1 | 0.8658 | 0.5657 | 0.6198 | 0.083* | |
C2 | 0.8626 (4) | 0.5573 (4) | 0.7514 (3) | 0.0814 (12) | |
H2 | 0.8990 | 0.4943 | 0.7650 | 0.098* | |
C3 | 0.8289 (4) | 0.6092 (5) | 0.8170 (3) | 0.0901 (14) | |
H3 | 0.8425 | 0.5829 | 0.8769 | 0.108* | |
C4 | 0.7734 (5) | 0.7029 (5) | 0.7927 (3) | 0.0888 (14) | |
H4 | 0.7516 | 0.7405 | 0.8372 | 0.107* | |
C5 | 0.7515 (4) | 0.7387 (3) | 0.7051 (3) | 0.0727 (11) | |
H5 | 0.7107 | 0.7992 | 0.6892 | 0.087* | |
C6 | 0.6742 (4) | 0.5249 (3) | 0.4540 (3) | 0.0719 (10) | |
H6 | 0.7489 | 0.5126 | 0.4857 | 0.086* | |
C7 | 0.6049 (5) | 0.4401 (4) | 0.4223 (4) | 0.0889 (14) | |
H7 | 0.6316 | 0.3732 | 0.4346 | 0.107* | |
C8 | 0.4944 (5) | 0.4594 (4) | 0.3717 (4) | 0.0958 (16) | |
H8 | 0.4458 | 0.4054 | 0.3472 | 0.115* | |
C9 | 0.4584 (5) | 0.5595 (4) | 0.3586 (4) | 0.0929 (14) | |
H9 | 0.3842 | 0.5742 | 0.3269 | 0.112* | |
C10 | 0.5322 (3) | 0.6369 (3) | 0.3925 (3) | 0.0737 (11) | |
H10 | 0.5068 | 0.7042 | 0.3810 | 0.088* | |
C11 | 0.9642 (3) | 0.6595 (2) | 0.4562 (2) | 0.0542 (8) |
U11 | U22 | U33 | U12 | U13 | U23 | |
V1 | 0.0328 (4) | 0.0368 (4) | 0.0389 (4) | 0.0019 (2) | 0.0126 (3) | −0.0020 (2) |
S1 | 0.0761 (7) | 0.0787 (7) | 0.1010 (9) | 0.0089 (5) | 0.0497 (6) | −0.0007 (5) |
N1 | 0.0552 (15) | 0.0657 (17) | 0.0553 (16) | −0.0015 (13) | 0.0173 (13) | −0.0020 (13) |
N2 | 0.0554 (15) | 0.0578 (16) | 0.0627 (17) | −0.0035 (13) | 0.0179 (13) | −0.0034 (13) |
N3 | 0.0551 (16) | 0.0685 (18) | 0.0692 (18) | 0.0064 (14) | 0.0228 (14) | −0.0023 (14) |
C1 | 0.071 (2) | 0.072 (2) | 0.065 (2) | 0.0113 (19) | 0.0213 (18) | 0.0083 (18) |
C2 | 0.074 (3) | 0.093 (3) | 0.076 (3) | 0.008 (2) | 0.020 (2) | 0.020 (2) |
C3 | 0.078 (3) | 0.126 (4) | 0.064 (2) | −0.004 (3) | 0.018 (2) | 0.024 (3) |
C4 | 0.089 (3) | 0.117 (4) | 0.067 (3) | −0.003 (3) | 0.034 (2) | −0.009 (3) |
C5 | 0.074 (3) | 0.083 (3) | 0.061 (2) | −0.0019 (19) | 0.020 (2) | −0.0114 (18) |
C6 | 0.072 (2) | 0.061 (2) | 0.085 (3) | −0.0012 (18) | 0.028 (2) | −0.0099 (18) |
C7 | 0.101 (4) | 0.063 (2) | 0.109 (4) | −0.011 (2) | 0.041 (3) | −0.013 (2) |
C8 | 0.102 (4) | 0.087 (3) | 0.105 (4) | −0.040 (3) | 0.042 (3) | −0.026 (3) |
C9 | 0.077 (3) | 0.095 (4) | 0.099 (3) | −0.019 (2) | 0.014 (3) | −0.018 (3) |
C10 | 0.060 (2) | 0.076 (2) | 0.081 (3) | −0.0013 (18) | 0.0147 (19) | −0.004 (2) |
C11 | 0.0569 (18) | 0.0493 (16) | 0.0559 (18) | 0.0040 (14) | 0.0156 (15) | −0.0010 (13) |
V1—N1 | 2.153 (3) | C2—H2 | 0.9300 |
V1—N2 | 2.173 (3) | C3—C4 | 1.396 (8) |
V1—N3 | 2.066 (3) | C3—H3 | 0.9300 |
V1—N3i | 2.066 (3) | C4—C5 | 1.345 (7) |
V1—N1i | 2.153 (3) | C4—H4 | 0.9300 |
V1—N2i | 2.173 (3) | C5—H5 | 0.9300 |
S1—C11 | 1.626 (4) | C6—C7 | 1.397 (6) |
N1—C5 | 1.346 (5) | C6—H6 | 0.9300 |
N1—C1 | 1.347 (5) | C7—C8 | 1.391 (9) |
N2—C6 | 1.329 (5) | C7—H7 | 0.9300 |
N2—C10 | 1.348 (5) | C8—C9 | 1.372 (7) |
N3—C11 | 1.160 (4) | C8—H8 | 0.9300 |
C1—C2 | 1.375 (6) | C9—C10 | 1.360 (6) |
C1—H1 | 0.9300 | C9—H9 | 0.9300 |
C2—C3 | 1.357 (8) | C10—H10 | 0.9300 |
N1—V1—N1i | 179.998 (1) | C1—C2—H2 | 121.0 |
N1—V1—N2 | 92.54 (11) | C2—C3—C4 | 118.8 (4) |
N1i—V1—N2 | 87.46 (11) | C2—C3—H3 | 120.6 |
N1—V1—N3 | 89.89 (12) | C4—C3—H3 | 120.6 |
N1i—V1—N3 | 90.11 (12) | C5—C4—C3 | 120.0 (5) |
N2—V1—N2i | 180.0 | C5—C4—H4 | 120.0 |
N2i—V1—N3 | 88.64 (12) | C3—C4—H4 | 120.0 |
N2—V1—N3 | 91.36 (12) | C4—C5—N1 | 122.3 (5) |
N3i—V1—N3 | 180.00 (17) | C4—C5—H5 | 118.9 |
N3i—V1—N1i | 89.89 (12) | N1—C5—H5 | 118.9 |
N3—V1—N1i | 90.11 (12) | N2—C6—C7 | 124.1 (5) |
N3i—V1—N2i | 91.36 (12) | N2—C6—H6 | 117.9 |
N3—V1—N2i | 88.64 (12) | C7—C6—H6 | 117.9 |
N1—V1—N2i | 87.46 (11) | C8—C7—C6 | 117.5 (5) |
N1i—V1—N2i | 92.54 (11) | C8—C7—H7 | 121.3 |
C5—N1—C1 | 116.8 (3) | C6—C7—H7 | 121.3 |
C5—N1—V1 | 121.2 (3) | C9—C8—C7 | 118.8 (4) |
C1—N1—V1 | 121.9 (2) | C9—C8—H8 | 120.6 |
C6—N2—C10 | 116.2 (3) | C7—C8—H8 | 120.6 |
C6—N2—V1 | 122.2 (3) | C10—C9—C8 | 119.3 (5) |
C10—N2—V1 | 121.6 (3) | C10—C9—H9 | 120.3 |
C11—N3—V1 | 156.6 (3) | C8—C9—H9 | 120.3 |
N1—C1—C2 | 124.0 (4) | N2—C10—C9 | 124.0 (4) |
N1—C1—H1 | 118.0 | N2—C10—H10 | 118.0 |
C2—C1—H1 | 118.0 | C9—C10—H10 | 118.0 |
C3—C2—C1 | 118.0 (4) | N3—C11—S1 | 179.0 (3) |
C3—C2—H2 | 121.0 |
Symmetry code: (i) −x+3/2, −y+3/2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
C5—H5···N3i | 0.93 | 2.53 | 3.064 (6) | 118 |
C1—H1···N3 | 0.93 | 2.56 | 3.090 (5) | 117 |
Symmetry code: (i) −x+3/2, −y+3/2, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [V(NCS)2(C5H5N)4] |
Mr | 483.50 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 273 |
a, b, c (Å) | 12.5011 (13), 13.003 (3), 14.999 (3) |
β (°) | 106.981 (5) |
V (Å3) | 2331.8 (8) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.63 |
Crystal size (mm) | 0.31 × 0.29 × 0.16 |
Data collection | |
Diffractometer | Bruker APEX-II area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.827, 0.904 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7623, 2332, 1933 |
Rint | 0.020 |
(sin θ/λ)max (Å−1) | 0.630 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.051, 0.178, 1.04 |
No. of reflections | 2332 |
No. of parameters | 143 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.34, −0.58 |
Computer programs: APEX2 (Bruker, 2005), SAINT (Siemens, 1996), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Siemens, 1996).
V1—N1 | 2.153 (3) | V1—N3 | 2.066 (3) |
V1—N2 | 2.173 (3) | ||
N1—V1—N1i | 179.998 (1) | N2—V1—N2i | 180.0 |
N1—V1—N2 | 92.54 (11) | N2i—V1—N3 | 88.64 (12) |
N1i—V1—N2 | 87.46 (11) | N2—V1—N3 | 91.36 (12) |
N1—V1—N3 | 89.89 (12) | N3i—V1—N3 | 180.00 (17) |
N1i—V1—N3 | 90.11 (12) |
Symmetry code: (i) −x+3/2, −y+3/2, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
C5—H5···N3i | 0.93 | 2.53 | 3.064 (6) | 118 |
C1—H1···N3 | 0.93 | 2.56 | 3.090 (5) | 117 |
Symmetry code: (i) −x+3/2, −y+3/2, −z+1. |
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The crystal structure of tetrakis(pyridine-κN)bis(thiocyanato- κN)chromium(II), (II), has previously been reported (Liu & Zhu, 2007). The crystal structure determination of the title compound, (I), has been carried out in order to elucidate the molecular conformation and to compare it with that of (II). We report herein the crystal structure of (I).
In the molecule of (I) (Fig. 1), the ligand bond lengths and angles (Table 1) are within normal ranges (Allen et al., 1987). The two N atoms of two SCN- and four N atoms of four pyridine ligands are coordinated to the V atom, in a distorted octahedral arrangement (Table 1). The V—N distances for the SCN- and pyridine ligand are 2.066 (3)Å and in the range of [2.153 (3)–2.173 (3) Å], respectively (Table 1), as in (II).
In the crystal structure, the C—H···N hydrogen bonds (Table 2, Fig. 2) result in the formation of a supramolecular network structure, as in (II). The both compounds, (I) and (II), are isostructural.