Chloro­[hydro­tris(pyrazol-1-yl)borato]oxo(1H-pyrazole)vanadium(IV)

The title compound, [V(C₉H₁₀BN₆)ClO(C₃H₄N₂)] or TpVOCl(pzH), exists in the solid state as discrete mol­ecules with V^IV in a psuedo-octa­hedral coordination geometry. The complex has three pyrazole units of the Tp ligand bound to one `face' of the vanadium center and chloro, oxo and pyrazole ligands bound to the other face. Bond lengths and angles are typical of structurally characterized complexes of known complexes of vanadium with substituted Tp ligands.

Key indicators

• Single-crystal X-ray study
• T = 100 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.073
• wR factor = 0.126
• Data-to-parameter ratio = 17.0

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         80
            C1  -N1  -V1  -O1    125.40  1.20   1.555   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         81
            N4  -N1  -V1  -O1    -55.20  1.30   1.555   1.555   1.555   1.555
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          1

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   3 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
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: CrysAlis CCD (Oxford Diffraction, 2004); cell refinement: CrysAlis RED (Oxford Diffraction, 2004); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXL97; software used to prepare material for publication: WinGX (Farrugia, 1999).

Chloro[hydrotris(pyrazol-1-yl)borato]oxo(1H-pyrazole)vanadium(IV)

Crystal data

[V(C9H10BN6)ClO(C3H4N2)]	F(000) = 780
Mr = 383.51	Dx = 1.583 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 7083 reflections
a = 8.3295 (5) Å	θ = 4.0–28.5°
b = 12.6110 (8) Å	µ = 0.80 mm^−1
c = 15.3711 (12) Å	T = 100 K
β = 94.642 (6)°	Prism, blue
V = 1609.34 (19) Å^3	0.07 × 0.05 × 0.02 mm
Z = 4

Data collection

Oxford Diffraction Xcalibur3 diffractometer equipped with a CCD detector	3685 independent reflections
Radiation source: Enhance (Mo) X-ray Source	3483 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.060
Detector resolution: 15.9890 pixels mm^-1	θmax = 27.5°, θmin = 4.1°
φ and ω scans	h = −10→10
Absorption correction: numerical Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark & Reid, 1995)	k = −16→16
Tmin = 0.901, Tmax = 0.962	l = −19→19
23290 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.074	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.126	H-atom parameters constrained
S = 1.24	w = 1/[σ^2(Fo^2) + (0.0298P)^2 + 3.4547P] where P = (Fo^2 + 2Fc^2)/3
3685 reflections	(Δ/σ)max < 0.001
217 parameters	Δρmax = 0.71 e Å^−3
0 restraints	Δρmin = −0.62 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
C1	0.4592 (4)	0.3287 (3)	0.0431 (2)	0.0246 (8)
H1	0.3877	0.3511	−0.0047	0.029*
C1P	0.0027 (5)	0.2357 (3)	−0.0651 (3)	0.0318 (9)
H1P	−0.0425	0.2517	−0.1223	0.038*
C2	0.6211 (4)	0.3032 (3)	0.0377 (2)	0.0250 (8)
H2	0.6795	0.3039	−0.0129	0.030*
C2P	0.0528 (5)	0.1386 (3)	−0.0343 (3)	0.0357 (9)
H2P1	0.0487	0.0733	−0.0652	0.043*
C3	0.6780 (4)	0.2767 (3)	0.1216 (2)	0.0204 (7)
H3	0.7852	0.2562	0.1398	0.025*
C3P	0.1106 (5)	0.1555 (3)	0.0513 (3)	0.0347 (9)
H3P	0.1553	0.1018	0.0892	0.042*
C4	0.1725 (4)	0.1162 (3)	0.2737 (2)	0.0236 (7)
H4	0.0600	0.1077	0.2601	0.028*
C5	0.2689 (4)	0.0447 (3)	0.3205 (2)	0.0242 (8)
H5	0.2373	−0.0206	0.3449	0.029*
C6	0.4209 (4)	0.0876 (3)	0.3247 (2)	0.0198 (7)
H6	0.5154	0.0566	0.3527	0.024*
C7	0.3324 (4)	0.5044 (3)	0.3277 (2)	0.0231 (7)
H7	0.2439	0.5519	0.3208	0.028*
C8	0.4679 (5)	0.5189 (3)	0.3864 (2)	0.0276 (8)
H8	0.4895	0.5760	0.4259	0.033*
C9	0.5641 (4)	0.4308 (3)	0.3736 (2)	0.0238 (8)
H9	0.6663	0.4166	0.4034	0.029*
B1	0.5452 (4)	0.2653 (3)	0.2711 (3)	0.0189 (8)
H1A	0.6515	0.2421	0.2997	0.023*
Cl1	0.15575 (10)	0.50236 (6)	0.10803 (6)	0.0233 (2)
N1	0.4191 (3)	0.3172 (2)	0.12504 (19)	0.0193 (6)
N1P	0.0958 (3)	0.2579 (2)	0.0744 (2)	0.0245 (7)
N2	0.2585 (3)	0.1994 (2)	0.24962 (19)	0.0204 (6)
N2P	0.0299 (3)	0.3044 (2)	0.0014 (2)	0.0263 (7)
H2P	0.0070	0.3724	−0.0025	0.032*
N3	0.3445 (3)	0.4151 (2)	0.28310 (19)	0.0199 (6)
N4	0.5553 (3)	0.2849 (2)	0.17325 (18)	0.0167 (6)
N5	0.4130 (3)	0.1811 (2)	0.28234 (19)	0.0186 (6)
N6	0.4876 (3)	0.3695 (2)	0.31211 (18)	0.0182 (6)
O1	0.0209 (3)	0.3479 (2)	0.23693 (17)	0.0276 (6)
V1	0.18486 (7)	0.34220 (5)	0.18852 (4)	0.02002 (16)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.0246 (18)	0.0283 (19)	0.0204 (18)	−0.0017 (15)	−0.0008 (14)	0.0065 (15)
C1P	0.029 (2)	0.035 (2)	0.031 (2)	−0.0009 (17)	0.0006 (16)	−0.0033 (17)
C2	0.0258 (18)	0.0270 (18)	0.0231 (19)	−0.0037 (15)	0.0066 (15)	0.0010 (15)
C2P	0.039 (2)	0.033 (2)	0.035 (2)	0.0007 (18)	−0.0001 (18)	−0.0089 (18)
C3	0.0184 (16)	0.0158 (16)	0.0271 (19)	−0.0012 (12)	0.0025 (14)	−0.0013 (14)
C3P	0.036 (2)	0.028 (2)	0.039 (2)	0.0024 (17)	−0.0045 (18)	−0.0031 (18)
C4	0.0214 (17)	0.0193 (17)	0.030 (2)	−0.0029 (13)	0.0046 (15)	0.0038 (15)
C5	0.0305 (19)	0.0168 (16)	0.0264 (19)	0.0000 (14)	0.0091 (16)	0.0019 (14)
C6	0.0259 (17)	0.0148 (15)	0.0188 (17)	0.0047 (13)	0.0018 (14)	0.0020 (13)
C7	0.0282 (18)	0.0178 (16)	0.0238 (18)	0.0040 (14)	0.0048 (15)	0.0038 (14)
C8	0.042 (2)	0.0198 (18)	0.0212 (18)	0.0006 (15)	0.0013 (16)	−0.0002 (14)
C9	0.0316 (19)	0.0209 (17)	0.0180 (17)	−0.0006 (14)	−0.0036 (14)	0.0024 (14)
B1	0.0173 (17)	0.0175 (18)	0.021 (2)	0.0008 (14)	−0.0023 (15)	0.0019 (15)
Cl1	0.0214 (4)	0.0187 (4)	0.0288 (5)	0.0014 (3)	−0.0030 (3)	0.0053 (3)
N1	0.0162 (13)	0.0211 (15)	0.0199 (15)	0.0001 (11)	−0.0028 (11)	0.0045 (11)
N1P	0.0192 (14)	0.0196 (14)	0.0340 (18)	−0.0007 (12)	−0.0024 (13)	0.0013 (13)
N2	0.0165 (13)	0.0180 (14)	0.0264 (16)	0.0010 (11)	−0.0001 (12)	0.0025 (12)
N2P	0.0238 (16)	0.0239 (15)	0.0306 (17)	−0.0014 (12)	−0.0019 (13)	−0.0008 (13)
N3	0.0206 (14)	0.0155 (14)	0.0240 (15)	0.0022 (11)	0.0043 (12)	0.0059 (11)
N4	0.0142 (13)	0.0140 (13)	0.0215 (15)	−0.0011 (10)	−0.0013 (11)	0.0004 (11)
N5	0.0154 (13)	0.0176 (14)	0.0225 (15)	0.0021 (11)	−0.0007 (11)	0.0021 (11)
N6	0.0200 (14)	0.0168 (13)	0.0175 (14)	0.0004 (11)	−0.0007 (11)	−0.0006 (11)
O1	0.0208 (12)	0.0293 (14)	0.0327 (15)	−0.0007 (10)	0.0022 (11)	0.0083 (11)
V1	0.0150 (3)	0.0178 (3)	0.0268 (3)	0.0008 (2)	−0.0012 (2)	0.0042 (2)

Geometric parameters (Å, º)

C1—N1	1.337 (5)	C7—C8	1.398 (5)
C1—C2	1.395 (5)	C7—H7	0.9500
C1—H1	0.9500	C8—C9	1.393 (5)
C1P—N2P	1.344 (5)	C8—H8	0.9500
C1P—C2P	1.367 (6)	C9—N6	1.342 (4)
C1P—H1P	0.9500	C9—H9	0.9500
C2—C3	1.378 (5)	B1—N4	1.533 (5)
C2—H2	0.9500	B1—N5	1.549 (5)
C2P—C3P	1.381 (6)	B1—N6	1.550 (5)
C2P—H2P1	0.9500	B1—H1A	1.0000
C3—N4	1.348 (4)	Cl1—V1	2.3708 (10)
C3—H3	0.9500	N1—N4	1.366 (4)
C3P—N1P	1.346 (5)	N1—V1	2.273 (3)
C3P—H3P	0.9500	N1P—N2P	1.343 (4)
C4—N2	1.339 (4)	N1P—V1	2.133 (3)
C4—C5	1.372 (5)	N2—N5	1.363 (4)
C4—H4	0.9500	N2—V1	2.100 (3)
C5—C6	1.373 (5)	N2P—H2P	0.8800
C5—H5	0.9500	N3—N6	1.365 (4)
C6—N5	1.347 (4)	N3—V1	2.101 (3)
C6—H6	0.9500	O1—V1	1.609 (3)
C7—N3	1.327 (4)
N1—C1—C2	110.3 (3)	N6—B1—H1A	111.2
N1—C1—H1	124.8	C1—N1—N4	106.5 (3)
C2—C1—H1	124.8	C1—N1—V1	132.7 (2)
N2P—C1P—C2P	106.7 (4)	N4—N1—V1	120.8 (2)
N2P—C1P—H1P	126.7	N2P—N1P—C3P	103.8 (3)
C2P—C1P—H1P	126.7	N2P—N1P—V1	124.1 (2)
C3—C2—C1	105.1 (3)	C3P—N1P—V1	131.4 (3)
C3—C2—H2	127.4	C4—N2—N5	106.0 (3)
C1—C2—H2	127.4	C4—N2—V1	130.7 (2)
C1P—C2P—C3P	105.3 (4)	N5—N2—V1	122.9 (2)
C1P—C2P—H2P1	127.4	N1P—N2P—C1P	112.7 (3)
C3P—C2P—H2P1	127.4	N1P—N2P—H2P	123.7
N4—C3—C2	108.2 (3)	C1P—N2P—H2P	123.7
N4—C3—H3	125.9	C7—N3—N6	106.8 (3)
C2—C3—H3	125.9	C7—N3—V1	131.2 (2)
N1P—C3P—C2P	111.5 (4)	N6—N3—V1	122.0 (2)
N1P—C3P—H3P	124.2	C3—N4—N1	109.8 (3)
C2P—C3P—H3P	124.2	C3—N4—B1	132.1 (3)
N2—C4—C5	110.9 (3)	N1—N4—B1	118.1 (3)
N2—C4—H4	124.6	C6—N5—N2	109.5 (3)
C5—C4—H4	124.6	C6—N5—B1	130.3 (3)
C4—C5—C6	105.3 (3)	N2—N5—B1	120.1 (3)
C4—C5—H5	127.3	C9—N6—N3	109.9 (3)
C6—C5—H5	127.3	C9—N6—B1	129.1 (3)
N5—C6—C5	108.3 (3)	N3—N6—B1	121.0 (3)
N5—C6—H6	125.9	O1—V1—N2	93.40 (12)
C5—C6—H6	125.9	O1—V1—N3	100.02 (13)
N3—C7—C8	110.7 (3)	N2—V1—N3	85.41 (11)
N3—C7—H7	124.6	O1—V1—N1P	98.67 (13)
C8—C7—H7	124.6	N2—V1—N1P	90.56 (11)
C9—C8—C7	104.4 (3)	N3—V1—N1P	161.07 (11)
C9—C8—H8	127.8	O1—V1—N1	174.28 (12)
C7—C8—H8	127.8	N2—V1—N1	81.00 (11)
N6—C9—C8	108.2 (3)	N3—V1—N1	80.81 (11)
N6—C9—H9	125.9	N1P—V1—N1	80.29 (11)
C8—C9—H9	125.9	O1—V1—Cl1	98.55 (10)
N4—B1—N5	108.4 (3)	N2—V1—Cl1	167.98 (8)
N4—B1—N6	107.8 (3)	N3—V1—Cl1	91.19 (8)
N5—B1—N6	106.8 (3)	N1P—V1—Cl1	88.94 (9)
N4—B1—H1A	111.2	N1—V1—Cl1	87.08 (8)
N5—B1—H1A	111.2
N1—C1—C2—C3	−0.7 (4)	N4—B1—N6—C9	−117.8 (4)
N2P—C1P—C2P—C3P	−0.7 (4)	N5—B1—N6—C9	125.8 (3)
C1—C2—C3—N4	0.8 (4)	N4—B1—N6—N3	58.2 (4)
C1P—C2P—C3P—N1P	1.0 (5)	N5—B1—N6—N3	−58.1 (4)
N2—C4—C5—C6	0.0 (4)	C4—N2—V1—O1	34.4 (3)
C4—C5—C6—N5	0.4 (4)	N5—N2—V1—O1	−137.3 (3)
N3—C7—C8—C9	0.1 (4)	C4—N2—V1—N3	134.2 (3)
C7—C8—C9—N6	−0.5 (4)	N5—N2—V1—N3	−37.5 (3)
C2—C1—N1—N4	0.4 (4)	C4—N2—V1—N1P	−64.3 (3)
C2—C1—N1—V1	179.9 (2)	N5—N2—V1—N1P	124.0 (3)
C2P—C3P—N1P—N2P	−0.8 (4)	C4—N2—V1—N1	−144.4 (3)
C2P—C3P—N1P—V1	−171.3 (3)	N5—N2—V1—N1	43.9 (3)
C5—C4—N2—N5	−0.4 (4)	C4—N2—V1—Cl1	−151.9 (3)
C5—C4—N2—V1	−173.2 (2)	N5—N2—V1—Cl1	36.4 (6)
C3P—N1P—N2P—C1P	0.4 (4)	C7—N3—V1—O1	−48.1 (3)
V1—N1P—N2P—C1P	171.7 (2)	N6—N3—V1—O1	129.1 (2)
C2P—C1P—N2P—N1P	0.2 (4)	C7—N3—V1—N2	−140.8 (3)
C8—C7—N3—N6	0.3 (4)	N6—N3—V1—N2	36.5 (2)
C8—C7—N3—V1	177.9 (2)	C7—N3—V1—N1P	141.0 (4)
C2—C3—N4—N1	−0.6 (4)	N6—N3—V1—N1P	−41.8 (5)
C2—C3—N4—B1	179.7 (3)	C7—N3—V1—N1	137.6 (3)
C1—N1—N4—C3	0.1 (4)	N6—N3—V1—N1	−45.1 (2)
V1—N1—N4—C3	−179.5 (2)	C7—N3—V1—Cl1	50.8 (3)
C1—N1—N4—B1	179.9 (3)	N6—N3—V1—Cl1	−132.0 (2)
V1—N1—N4—B1	0.4 (4)	N2P—N1P—V1—O1	88.4 (3)
N5—B1—N4—C3	−122.8 (4)	C3P—N1P—V1—O1	−102.8 (4)
N6—B1—N4—C3	121.9 (3)	N2P—N1P—V1—N2	−178.0 (3)
N5—B1—N4—N1	57.5 (4)	C3P—N1P—V1—N2	−9.3 (4)
N6—B1—N4—N1	−57.8 (4)	N2P—N1P—V1—N3	−100.6 (4)
C5—C6—N5—N2	−0.7 (4)	C3P—N1P—V1—N3	68.1 (5)
C5—C6—N5—B1	176.3 (3)	N2P—N1P—V1—N1	−97.3 (3)
C4—N2—N5—C6	0.7 (4)	C3P—N1P—V1—N1	71.5 (4)
V1—N2—N5—C6	174.2 (2)	N2P—N1P—V1—Cl1	−10.1 (3)
C4—N2—N5—B1	−176.7 (3)	C3P—N1P—V1—Cl1	158.7 (3)
V1—N2—N5—B1	−3.2 (4)	C1—N1—V1—O1	125.4 (12)
N4—B1—N5—C6	124.2 (4)	N4—N1—V1—O1	−55.2 (13)
N6—B1—N5—C6	−119.8 (4)	C1—N1—V1—N2	137.4 (3)
N4—B1—N5—N2	−59.0 (4)	N4—N1—V1—N2	−43.2 (2)
N6—B1—N5—N2	56.9 (4)	C1—N1—V1—N3	−135.8 (3)
C8—C9—N6—N3	0.7 (4)	N4—N1—V1—N3	43.6 (2)
C8—C9—N6—B1	177.1 (3)	C1—N1—V1—N1P	45.3 (3)
C7—N3—N6—C9	−0.6 (4)	N4—N1—V1—N1P	−135.3 (2)
V1—N3—N6—C9	−178.5 (2)	C1—N1—V1—Cl1	−44.1 (3)
C7—N3—N6—B1	−177.4 (3)	N4—N1—V1—Cl1	135.2 (2)
V1—N3—N6—B1	4.8 (4)