Low-temperature oxobis(2,2,6,6-tetra­methyl-3,5-heptanedionato)­vanadium(IV)

The coordination geometry around the V atom in the title complex, [VO(C₁₁H₁₉O₂)₂], is square pyramidal with the basal plane defined by four O atoms from two chelating β-diketonate ligands and the axial position occupied by an oxo group.

Key indicators

• Single-crystal X-ray study
• T = 149 K
• Mean [sigma](C-C) = 0.010 Å
• Disorder in main residue
• R factor = 0.074
• wR factor = 0.187
• Data-to-parameter ratio = 16.0

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


 Alert Level B:



PLAT_213  Alert B Atom  C18    has ADP max/min Ratio ...........       4.40


 Alert Level C:



PLAT_213  Alert C Atom  C22    has ADP max/min Ratio ...........       3.10

PLAT_301  Alert C Main Residue Disorder ........................      10.00 Perc.

General Notes



REFLT_03
         From the CIF: _diffrn_reflns_theta_max           26.50
         From the CIF: _reflns_number_total               4217
         Count of symmetry unique reflns         2689
         Completeness (_total/calc)            156.82%
         TEST3: Check Friedels for noncentro structure
         Estimate of Friedel pairs measured      1528
         Fraction of Friedel pairs measured     0.568
         Are heavy atom types Z>Si present          yes
          Please check that the estimate of the number of Friedel pairs is
          correct. If it is not, please give the correct count in the
          _publ_section_exptl_refinement section of the submitted CIF.


 0 Alert Level A = Potentially serious problem

 1 Alert Level B = Potential problem

 2 Alert Level C = Please check

---

Computing details

Data collection: XSCANS (Fait, 1991); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXS86 (Sheldrick, 1985); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Johnson, 1976; Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

oxobis(2,2,6,6-tetramethyl-3,5-heptadionato)vanadium(IV)

Crystal data

[VO(C11H19O2)2]	F(000) = 466
Mr = 433.46	Dx = 1.171 Mg m^−3
Monoclinic, P21	Mo Kα radiation, λ = 0.71073 Å
a = 9.4515 (2) Å	Cell parameters from 25 reflections
b = 10.7953 (3) Å	θ = 8–15°
c = 12.7494 (4) Å	µ = 0.43 mm^−1
β = 109.025 (1)°	T = 149 K
V = 1229.79 (6) Å^3	Prism, green
Z = 2	0.50 × 0.40 × 0.40 mm

Data collection

Siemens P4 diffractometer	Rint = 0.093
Radiation source: fine-focus sealed tube	θmax = 26.5°, θmin = 1.7°
Graphite monochromator	h = −11→11
ω scans	k = −9→13
7897 measured reflections	l = −15→14
4217 independent reflections	3 standard reflections every 120 min
2751 reflections with I > 2σ(I)	intensity decay: no decay

Refinement

Refinement on F^2	H atoms treated by a mixture of independent and constrained refinement
Least-squares matrix: full	w = 1/[σ^2(Fo^2) + (0.0898P)^2] where P = (Fo^2 + 2Fc^2)/3
R[F^2 > 2σ(F^2)] = 0.074	(Δ/σ)max < 0.001
wR(F^2) = 0.187	Δρmax = 0.95 e Å^−3
S = 0.92	Δρmin = −1.01 e Å^−3
4217 reflections	Absolute structure: Flack (1983)
263 parameters	Absolute structure parameter: 0.03 (5)
1 restraint

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
V1	0.71881 (10)	0.26486 (9)	0.31402 (8)	0.0238 (3)
O2	0.6290 (4)	0.1734 (4)	0.4098 (3)	0.0278 (10)
O4	0.8731 (4)	0.2700 (5)	0.2425 (3)	0.0295 (9)
O1	0.8863 (5)	0.3000 (4)	0.4482 (3)	0.0306 (12)
O3	0.6198 (4)	0.1396 (4)	0.2014 (3)	0.0272 (11)
C1	0.8940 (6)	0.2958 (5)	0.5501 (5)	0.0230 (15)
C15	0.5284 (7)	0.0200 (6)	0.0366 (5)	0.0246 (15)
C19	0.9992 (6)	0.2808 (8)	0.1103 (5)	0.0328 (16)
C18	0.6081 (8)	−0.0684 (6)	−0.0209 (6)	0.0353 (17)
H18A	0.6418	−0.0227	−0.0729	0.053*
H18B	0.5396	−0.1318	−0.0595	0.053*
H18C	0.6924	−0.1058	0.0338	0.053*
C12	0.8661 (6)	0.2364 (5)	0.1459 (5)	0.0196 (14)
C3	0.6589 (7)	0.1788 (6)	0.5143 (5)	0.0235 (14)
C13	0.7560 (6)	0.1642 (6)	0.0780 (5)	0.0236 (14)
H13	0.7579	0.1482	0.0068	0.028*
C8	1.0346 (7)	0.3479 (7)	0.6322 (6)	0.0334 (17)
C4	0.5548 (7)	0.1020 (6)	0.5605 (5)	0.0265 (15)
C2	0.7811 (6)	0.2412 (6)	0.5838 (5)	0.0296 (17)
H2	0.7893	0.2474	0.6583	0.035*
C14	0.6381 (6)	0.1118 (6)	0.1100 (5)	0.0206 (13)
C17	0.4572 (9)	−0.0566 (7)	0.1066 (6)	0.044 (2)
H17A	0.5325	−0.1066	0.1579	0.066*
H17B	0.3812	−0.1092	0.0591	0.066*
H17C	0.4131	−0.0023	0.147	0.066*
C7	0.3971 (8)	0.1048 (8)	0.4806 (7)	0.051 (2)
H7A	0.3349	0.0517	0.5074	0.077*
H7B	0.3966	0.0765	0.4091	0.077*
H7C	0.3594	0.188	0.4744	0.077*
O5	0.6249 (5)	0.3889 (4)	0.2791 (4)	0.0401 (13)
C6	0.6123 (9)	−0.0323 (7)	0.5697 (8)	0.056 (3)
H6A	0.554	−0.0832	0.6019	0.084*
H6B	0.7154	−0.0345	0.6158	0.084*
H6C	0.6035	−0.0629	0.4972	0.084*
C16	0.4075 (8)	0.0918 (7)	−0.0501 (6)	0.045 (2)
H16A	0.3578	0.1464	−0.0139	0.068*
H16B	0.3361	0.0349	−0.0965	0.068*
H16C	0.452	0.1394	−0.0947	0.068*
C5	0.5558 (9)	0.1487 (8)	0.6727 (6)	0.051 (2)
H5A	0.5334	0.2357	0.668	0.077*
H5B	0.6528	0.1351	0.7264	0.077*
H5C	0.4817	0.1049	0.6949	0.077*
C21	1.1383 (8)	0.2221 (8)	0.1837 (8)	0.061 (3)
H21A	1.1345	0.1345	0.1701	0.092*
H21B	1.1473	0.2371	0.2598	0.092*
H21C	1.2232	0.2567	0.1686	0.092*
C20	1.0133 (9)	0.4237 (7)	0.1325 (8)	0.058 (2)
H20A	1.0186	0.4398	0.2077	0.087*
H20B	0.9276	0.4649	0.0828	0.087*
H20C	1.1024	0.4539	0.1207	0.087*
C22	0.9772 (9)	0.2583 (12)	−0.0111 (6)	0.072 (3)
H22A	1.0551	0.2993	−0.0309	0.109*
H22B	0.8817	0.2904	−0.0555	0.109*
H22C	0.9809	0.171	−0.0241	0.109*
C9A	1.1227 (15)	0.2348 (14)	0.7071 (12)	0.060 (3)*	0.580 (7)
H9A1	1.2182	0.2632	0.7549	0.089*	0.580 (7)
H9A2	1.1372	0.1701	0.66	0.089*	0.580 (7)
H9A3	1.0654	0.2035	0.7511	0.089*	0.580 (7)
C10A	0.9955 (15)	0.4329 (15)	0.7119 (12)	0.048 (3)*	0.580 (7)
H10A	0.9496	0.386	0.7561	0.072*	0.580 (7)
H10B	0.927	0.4952	0.6711	0.072*	0.580 (7)
H10C	1.0847	0.4718	0.7593	0.072*	0.580 (7)
C11A	1.1368 (16)	0.4022 (15)	0.5784 (13)	0.056 (3)*	0.580 (7)
H11A	1.0932	0.4765	0.5398	0.084*	0.580 (7)
H11B	1.1528	0.3439	0.5265	0.084*	0.580 (7)
H11C	1.2307	0.4216	0.6337	0.084*	0.580 (7)
C10B	1.1622 (16)	0.267 (2)	0.6225 (14)	0.048 (3)*	0.420 (7)
H10D	1.2551	0.2948	0.6746	0.072*	0.420 (7)
H10E	1.1671	0.2729	0.5486	0.072*	0.420 (7)
H10F	1.1448	0.1824	0.6381	0.072*	0.420 (7)
C11B	1.033 (2)	0.358 (2)	0.7442 (17)	0.056 (3)*	0.420 (7)
H11D	1.1244	0.397	0.7892	0.084*	0.420 (7)
H11E	1.0258	0.2772	0.7728	0.084*	0.420 (7)
H11F	0.9494	0.4075	0.7454	0.084*	0.420 (7)
C9B	1.055 (2)	0.482 (2)	0.5859 (18)	0.060 (3)*	0.420 (7)
H9B1	0.9805	0.5375	0.5954	0.089*	0.420 (7)
H9B2	1.0442	0.4765	0.5085	0.089*	0.420 (7)
H9B3	1.1528	0.5137	0.6261	0.089*	0.420 (7)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
V1	0.0401 (5)	0.0192 (5)	0.0170 (5)	−0.0041 (5)	0.0160 (4)	−0.0037 (6)
O2	0.043 (2)	0.027 (3)	0.018 (3)	−0.011 (2)	0.015 (2)	−0.007 (2)
O4	0.043 (2)	0.032 (3)	0.018 (2)	−0.010 (3)	0.0168 (17)	−0.009 (3)
O1	0.044 (2)	0.031 (3)	0.023 (2)	−0.016 (2)	0.021 (2)	−0.0082 (19)
O3	0.039 (2)	0.028 (3)	0.020 (2)	−0.0117 (19)	0.016 (2)	−0.008 (2)
C1	0.040 (3)	0.018 (4)	0.016 (3)	0.004 (3)	0.015 (3)	−0.001 (2)
C15	0.041 (4)	0.018 (4)	0.017 (4)	−0.002 (3)	0.012 (3)	−0.008 (3)
C19	0.041 (3)	0.036 (5)	0.028 (3)	−0.004 (4)	0.021 (3)	−0.006 (4)
C18	0.059 (5)	0.016 (4)	0.035 (4)	−0.009 (3)	0.021 (4)	−0.020 (3)
C12	0.034 (3)	0.010 (4)	0.015 (3)	0.004 (2)	0.008 (2)	0.000 (2)
C3	0.037 (3)	0.018 (3)	0.021 (4)	0.004 (3)	0.016 (3)	0.006 (3)
C13	0.038 (3)	0.022 (4)	0.014 (3)	−0.003 (3)	0.013 (3)	−0.006 (3)
C8	0.042 (4)	0.035 (4)	0.025 (4)	−0.012 (3)	0.014 (3)	−0.009 (3)
C4	0.043 (4)	0.022 (4)	0.022 (4)	−0.007 (3)	0.020 (3)	−0.002 (3)
C2	0.043 (3)	0.034 (5)	0.015 (3)	−0.006 (3)	0.015 (3)	−0.001 (3)
C14	0.033 (3)	0.015 (3)	0.017 (3)	0.003 (2)	0.012 (3)	0.004 (3)
C17	0.069 (5)	0.030 (5)	0.039 (5)	−0.024 (4)	0.026 (4)	−0.009 (4)
C7	0.054 (5)	0.045 (5)	0.065 (6)	−0.009 (4)	0.035 (5)	0.013 (5)
O5	0.067 (3)	0.025 (3)	0.033 (3)	0.014 (2)	0.023 (3)	0.011 (2)
C6	0.065 (5)	0.032 (5)	0.086 (7)	0.007 (4)	0.046 (5)	0.021 (5)
C16	0.043 (4)	0.032 (5)	0.049 (5)	0.003 (3)	−0.004 (4)	−0.007 (4)
C5	0.074 (5)	0.048 (5)	0.045 (5)	−0.026 (4)	0.038 (4)	−0.004 (4)
C21	0.053 (5)	0.046 (6)	0.093 (7)	0.006 (4)	0.036 (5)	0.022 (5)
C20	0.065 (5)	0.030 (5)	0.095 (7)	−0.005 (4)	0.048 (5)	0.008 (5)
C22	0.082 (5)	0.100 (7)	0.063 (5)	−0.046 (7)	0.061 (5)	−0.035 (7)

Geometric parameters (Å, º)

V1—O5	1.588 (5)	C19—C22	1.513 (9)
V1—O1	1.952 (4)	C19—C12	1.546 (7)
V1—O4	1.957 (3)	C19—C20	1.566 (11)
V1—O2	1.965 (4)	C12—C13	1.361 (8)
V1—O3	1.972 (4)	C3—C2	1.381 (8)
O2—C3	1.270 (7)	C3—C4	1.543 (8)
O4—C12	1.264 (6)	C13—C14	1.423 (8)
O1—C1	1.279 (7)	C8—C11B	1.44 (2)
O3—C14	1.269 (7)	C8—C11A	1.476 (15)
C1—C2	1.403 (8)	C8—C10A	1.502 (15)
C1—C8	1.507 (8)	C8—C10B	1.526 (19)
C15—C14	1.516 (8)	C8—C9B	1.60 (2)
C15—C16	1.518 (9)	C8—C9A	1.605 (16)
C15—C17	1.526 (8)	C4—C7	1.506 (10)
C15—C18	1.541 (8)	C4—C5	1.514 (9)
C19—C21	1.485 (10)	C4—C6	1.539 (10)
O5—V1—O1	107.5 (2)	C2—C3—C4	121.4 (5)
O5—V1—O4	106.2 (2)	C12—C13—C14	123.6 (5)
O1—V1—O4	83.59 (16)	C11B—C8—C11A	130.5 (12)
O5—V1—O2	106.4 (2)	C11B—C8—C10A	36.5 (10)
O1—V1—O2	86.81 (16)	C11A—C8—C10A	114.5 (10)
O4—V1—O2	147.4 (2)	C11B—C8—C1	115.4 (10)
O5—V1—O3	106.6 (2)	C11A—C8—C1	112.8 (8)
O1—V1—O3	145.88 (18)	C10A—C8—C1	109.9 (7)
O4—V1—O3	85.92 (18)	C11B—C8—C10B	112.8 (12)
O2—V1—O3	84.78 (17)	C11A—C8—C10B	62.3 (11)
C3—O2—V1	129.5 (4)	C10A—C8—C10B	141.3 (10)
C12—O4—V1	129.5 (3)	C1—C8—C10B	105.8 (8)
C1—O1—V1	130.2 (4)	C11B—C8—C9B	109.7 (14)
C14—O3—V1	131.0 (4)	C11A—C8—C9B	45.0 (9)
O1—C1—C2	121.9 (6)	C10A—C8—C9B	77.4 (10)
O1—C1—C8	115.9 (5)	C1—C8—C9B	105.5 (9)
C2—C1—C8	122.1 (5)	C10B—C8—C9B	107.2 (12)
C14—C15—C16	108.5 (5)	C11B—C8—C9A	68.8 (11)
C14—C15—C17	109.6 (5)	C11A—C8—C9A	106.7 (9)
C16—C15—C17	109.4 (6)	C10A—C8—C9A	104.9 (9)
C14—C15—C18	110.9 (5)	C1—C8—C9A	107.4 (7)
C16—C15—C18	109.8 (5)	C10B—C8—C9A	48.9 (8)
C17—C15—C18	108.6 (6)	C9B—C8—C9A	143.8 (10)
C21—C19—C22	112.0 (7)	C7—C4—C5	109.4 (6)
C21—C19—C12	108.7 (6)	C7—C4—C6	108.5 (6)
C22—C19—C12	113.4 (5)	C5—C4—C6	110.4 (7)
C21—C19—C20	107.5 (6)	C7—C4—C3	110.2 (5)
C22—C19—C20	108.6 (8)	C5—C4—C3	111.9 (5)
C12—C19—C20	106.3 (5)	C6—C4—C3	106.4 (5)
O4—C12—C13	124.7 (5)	C3—C2—C1	124.7 (5)
O4—C12—C19	114.1 (5)	O3—C14—C13	121.6 (5)
C13—C12—C19	121.1 (5)	O3—C14—C15	116.8 (5)
O2—C3—C2	123.3 (5)	C13—C14—C15	121.6 (5)
O2—C3—C4	115.1 (5)