Oxotris­(quinolin-8-olato-κ²O,N)­tantalum(V) di­chloro­methane disolvate

The Ta^V atom in the title compound, [Ta(C₉H₆NO)₃O]·2CH₂Cl₂, is chelated by three quinolin-8-olate ligands and exists in a pentagonal–bipramidal geometry. The Ta and oxo O atoms and one of the quinolin-8-olate ligands lie on a mirror plane that relates the other two quinolin-8-olate ligands to one another. The compound is isostructural with the Nb^V di­chloro­methane disolvate reported by Amini, Mirzaee, Yeganeh & Ng [Acta Cryst. (2004), E60, m147–m148].

Key indicators

• Single-crystal X-ray study
• T = 93 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.024
• wR factor = 0.064
• Data-to-parameter ratio = 14.5

checkCIF/PLATON results

No syntax errors found



Alert level B
ABSTM02_ALERT_3_B  The ratio of expected to reported Tmax/Tmin(RR') is < 0.75
            Tmin and Tmax reported:      0.189     0.376
            Tmin' and Tmax expected:      0.235     0.296
            RR' =      0.635
            Please check that your absorption correction is appropriate.
PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large .............       0.55

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.79

Alert level G
ABSTM02_ALERT_3_G  When printed, the submitted absorption T values will be
            replaced by the scaled T values. Since the ratio of scaled T's
            is identical to the ratio of reported T values, the scaling
            does not imply a change to the absorption corrections used in
            the study.
            Ratio of Tmax expected/reported      0.789
            Tmax scaled      0.296 Tmin scaled      0.149

   0 ALERT level A = In general: serious problem
   2 ALERT level B = Potentially serious problem
   2 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   1 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
   3 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: atomic coordinates taken from the isostructural Nb analog; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.

Oxotris(quinolin-8-olato-κ²O,N)tantalum(V) dichloromethane disolvate

Crystal data

[Ta(C9H6NO)3O]·2CH2Cl2	F(000) = 1560
Mr = 799.25	Dx = 1.893 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 8025 reflections
a = 12.4473 (5) Å	θ = 2.6–26.5°
b = 17.4957 (7) Å	µ = 4.34 mm^−1
c = 12.8805 (5) Å	T = 93 K
V = 2805.0 (2) Å^3	Block, yellow
Z = 4	0.32 × 0.30 × 0.28 mm

Data collection

Siemens P4/CCD area-detector diffractometer	2975 independent reflections
Radiation source: medium-focus sealed tube	2718 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.035
φ and ω scans	θmax = 26.5°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 2001)	h = −15→15
Tmin = 0.189, Tmax = 0.376	k = −21→21
21960 measured reflections	l = −16→16

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)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.064	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.0405P)^2 + 4.9159P] where P = (Fo^2 + 2Fc^2)/3
2975 reflections	(Δ/σ)max = 0.001
205 parameters	Δρmax = 1.78 e Å^−3
0 restraints	Δρmin = −2.29 e Å^−3

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

	x	y	z	Uiso*/Ueq
Ta1	0.127955 (12)	0.2500	0.016576 (12)	0.00793 (8)
Cl1	0.52844 (8)	0.40631 (5)	−0.07483 (7)	0.0319 (2)
Cl2	0.44429 (8)	0.36744 (5)	0.12880 (7)	0.0348 (2)
O1	0.2580 (2)	0.2500	−0.0345 (2)	0.0132 (6)
O2	0.13971 (16)	0.31858 (11)	0.14374 (16)	0.0127 (4)
O3	0.0460 (2)	0.2500	−0.1213 (2)	0.0106 (6)
N1	0.1134 (2)	0.37760 (15)	−0.0365 (2)	0.0108 (5)
N2	−0.0568 (3)	0.2500	0.0563 (3)	0.0089 (6)
C1	0.0978 (2)	0.40495 (17)	−0.1306 (2)	0.0136 (6)
H1	0.0822	0.3703	−0.1854	0.016*
C2	0.1034 (3)	0.48414 (17)	−0.1531 (3)	0.0170 (6)
H2	0.0908	0.5019	−0.2217	0.020*
C3	0.1269 (2)	0.53462 (18)	−0.0758 (3)	0.0169 (7)
H3	0.1320	0.5877	−0.0906	0.020*
C4	0.1437 (3)	0.50789 (19)	0.0262 (3)	0.0143 (7)
C5	0.1647 (2)	0.55368 (17)	0.1143 (3)	0.0183 (6)
H5	0.1722	0.6075	0.1071	0.022*
C6	0.1740 (2)	0.52043 (17)	0.2097 (3)	0.0180 (6)
H6	0.1864	0.5521	0.2683	0.022*
C7	0.1660 (2)	0.44035 (17)	0.2245 (2)	0.0160 (6)
H7	0.1731	0.4188	0.2919	0.019*
C8	0.1480 (2)	0.39465 (16)	0.1402 (2)	0.0122 (6)
C9	0.1351 (2)	0.42851 (17)	0.0418 (3)	0.0115 (6)
C10	−0.1052 (4)	0.2500	0.1478 (4)	0.0150 (8)
H10	−0.0624	0.2500	0.2089	0.018*
C11	−0.2180 (4)	0.2500	0.1580 (4)	0.0171 (9)
H11	−0.2501	0.2500	0.2249	0.021*
C12	−0.2802 (4)	0.2500	0.0715 (4)	0.0179 (9)
H12	−0.3562	0.2500	0.0779	0.021*
C13	−0.2324 (4)	0.2500	−0.0281 (3)	0.0126 (8)
C14	−0.2879 (3)	0.2500	−0.1241 (4)	0.0157 (9)
H14	−0.3642	0.2500	−0.1251	0.019*
C15	−0.2316 (3)	0.2500	−0.2152 (3)	0.0151 (8)
H15	−0.2701	0.2500	−0.2789	0.018*
C16	−0.1179 (3)	0.2500	−0.2181 (4)	0.0127 (8)
H16	−0.0812	0.2500	−0.2827	0.015*
C17	−0.0610 (3)	0.2500	−0.1260 (3)	0.0096 (8)
C18	−0.1187 (3)	0.2500	−0.0315 (3)	0.0096 (8)
C19	0.4116 (3)	0.3939 (2)	0.0011 (3)	0.0233 (7)
H19A	0.3701	0.4422	0.0021	0.028*
H19B	0.3659	0.3539	−0.0306	0.028*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ta1	0.00816 (11)	0.00608 (11)	0.00954 (11)	0.000	−0.00150 (5)	0.000
Cl1	0.0345 (5)	0.0268 (4)	0.0345 (5)	−0.0004 (4)	0.0115 (4)	0.0003 (4)
Cl2	0.0433 (6)	0.0334 (5)	0.0276 (4)	−0.0015 (4)	0.0064 (4)	0.0000 (4)
O1	0.0125 (15)	0.0093 (14)	0.0177 (15)	0.000	−0.0017 (12)	0.000
O2	0.0187 (11)	0.0066 (10)	0.0128 (11)	−0.0009 (8)	−0.0049 (8)	−0.0005 (8)
O3	0.0092 (14)	0.0125 (13)	0.0102 (13)	0.000	−0.0008 (11)	0.000
N1	0.0098 (11)	0.0067 (12)	0.0159 (13)	0.0003 (9)	0.0010 (9)	0.0025 (9)
N2	0.0104 (16)	0.0071 (15)	0.0093 (16)	0.000	0.0026 (13)	0.000
C1	0.0116 (14)	0.0130 (14)	0.0160 (15)	0.0007 (11)	0.0016 (11)	0.0022 (11)
C2	0.0157 (15)	0.0151 (14)	0.0201 (16)	0.0044 (12)	0.0043 (12)	0.0091 (12)
C3	0.0134 (15)	0.0103 (15)	0.0270 (18)	0.0005 (10)	0.0036 (12)	0.0047 (13)
C4	0.0073 (13)	0.0092 (15)	0.0264 (19)	0.0013 (11)	0.0014 (11)	0.0008 (11)
C5	0.0122 (14)	0.0085 (13)	0.0341 (18)	−0.0013 (12)	−0.0025 (13)	−0.0030 (12)
C6	0.0143 (15)	0.0115 (14)	0.0281 (17)	0.0005 (11)	−0.0061 (13)	−0.0072 (12)
C7	0.0143 (15)	0.0141 (14)	0.0197 (16)	0.0016 (12)	−0.0065 (12)	−0.0012 (11)
C8	0.0107 (13)	0.0068 (13)	0.0192 (16)	0.0017 (10)	−0.0018 (11)	−0.0013 (11)
C9	0.0091 (14)	0.0060 (14)	0.0195 (15)	−0.0009 (10)	0.0005 (11)	−0.0018 (12)
C10	0.022 (2)	0.0108 (19)	0.013 (2)	0.000	0.0017 (17)	0.000
C11	0.019 (2)	0.014 (2)	0.018 (2)	0.000	0.0088 (18)	0.000
C12	0.016 (2)	0.0111 (19)	0.027 (3)	0.000	0.0111 (18)	0.000
C13	0.011 (2)	0.0059 (19)	0.021 (2)	0.000	0.0010 (16)	0.000
C14	0.009 (2)	0.0107 (19)	0.027 (2)	0.000	−0.0049 (17)	0.000
C15	0.015 (2)	0.0120 (19)	0.019 (2)	0.000	−0.0083 (17)	0.000
C16	0.015 (2)	0.0097 (18)	0.014 (2)	0.000	−0.0010 (15)	0.000
C17	0.0111 (19)	0.0047 (17)	0.0130 (19)	0.000	0.0000 (15)	0.000
C18	0.012 (2)	0.0047 (19)	0.012 (2)	0.000	0.0002 (15)	0.000
C19	0.0150 (17)	0.0211 (18)	0.0337 (19)	−0.0033 (14)	−0.0006 (14)	−0.0025 (14)

Geometric parameters (Å, º)

Ta1—O1	1.747 (3)	C5—H5	0.9500
Ta1—O2	2.036 (2)	C6—C7	1.418 (4)
Ta1—O2^i	2.036 (2)	C6—H6	0.9500
Ta1—O3	2.049 (3)	C7—C8	1.367 (4)
Ta1—N1^i	2.342 (3)	C7—H7	0.9500
Ta1—N1	2.342 (3)	C8—C9	1.409 (5)
Ta1—N2	2.356 (3)	C10—C11	1.409 (6)
Cl1—C19	1.766 (4)	C10—H10	0.9500
Cl2—C19	1.757 (4)	C11—C12	1.357 (7)
O2—C8	1.336 (3)	C11—H11	0.9500
O3—C17	1.332 (5)	C12—C13	1.414 (6)
N1—C1	1.318 (4)	C12—H12	0.9500
N1—C9	1.372 (4)	C13—C18	1.417 (6)
N2—C10	1.324 (6)	C13—C14	1.416 (6)
N2—C18	1.369 (5)	C14—C15	1.367 (6)
C1—C2	1.417 (4)	C14—H14	0.9500
C1—H1	0.9500	C15—C16	1.415 (6)
C2—C3	1.363 (5)	C15—H15	0.9500
C2—H2	0.9500	C16—C17	1.382 (6)
C3—C4	1.411 (5)	C16—H16	0.9500
C3—H3	0.9500	C17—C18	1.414 (6)
C4—C9	1.407 (4)	C19—H19A	0.9900
C4—C5	1.412 (5)	C19—H19B	0.9900
C5—C6	1.365 (5)
O1—Ta1—O2	103.7 (1)	C5—C6—H6	118.8
O1—Ta1—O2^i	103.7 (1)	C7—C6—H6	118.8
O1—Ta1—O3	97.8 (1)	C8—C7—C6	118.8 (3)
O1—Ta1—N1	87.8 (1)	C8—C7—H7	120.6
O1—Ta1—N1^i	87.8 (1)	C6—C7—H7	120.6
O1—Ta1—N2	170.4 (1)	O2—C8—C7	124.7 (3)
O2—Ta1—O2^i	72.2 (1)	O2—C8—C9	116.1 (3)
O2—Ta1—O3	137.2 (1)	C7—C8—C9	119.2 (3)
O2—Ta1—N1^i	143.4 (1)	N1—C9—C4	123.5 (3)
O2—Ta1—N1	71.2 (1)	N1—C9—C8	114.2 (3)
O2—Ta1—N2	84.0 (1)	C4—C9—C8	122.3 (3)
O2^i—Ta1—O3	137.2 (1)	N2—C10—C11	122.4 (4)
O2^i—Ta1—N1^i	71.2 (1)	N2—C10—H10	118.8
O2^i—Ta1—N1	143.4 (1)	C11—C10—H10	118.8
O2^i—Ta1—N2	84.0 (1)	C12—C11—C10	119.5 (4)
O3—Ta1—N1	73.1 (1)	C12—C11—H11	120.2
O3—Ta1—N1^i	73.1 (1)	C10—C11—H11	120.2
O3—Ta1—N2	72.7 (1)	C11—C12—C13	120.3 (4)
N1^i—Ta1—N1	144.9 (1)	C11—C12—H12	119.8
N1—Ta1—N2	89.3 (1)	C13—C12—H12	119.8
N1^i—Ta1—N2	89.3 (1)	C12—C13—C18	116.6 (4)
C8—O2—Ta1	124.5 (2)	C12—C13—C14	126.0 (4)
C17—O3—Ta1	122.5 (3)	C18—C13—C14	117.4 (4)
C1—N1—C9	118.0 (3)	C15—C14—C13	120.0 (4)
C1—N1—Ta1	128.8 (2)	C15—C14—H14	120.0
C9—N1—Ta1	112.9 (2)	C13—C14—H14	120.0
C10—N2—C18	118.6 (4)	C14—C15—C16	122.4 (4)
C10—N2—Ta1	129.7 (3)	C14—C15—H15	118.8
C18—N2—Ta1	111.7 (3)	C16—C15—H15	118.8
N1—C1—C2	122.4 (3)	C17—C16—C15	119.4 (4)
N1—C1—H1	118.8	C17—C16—H16	120.3
C2—C1—H1	118.8	C15—C16—H16	120.3
C3—C2—C1	119.7 (3)	O3—C17—C16	123.5 (4)
C3—C2—H2	120.2	O3—C17—C18	117.9 (4)
C1—C2—H2	120.2	C16—C17—C18	118.6 (4)
C2—C3—C4	119.8 (3)	N2—C18—C17	115.2 (4)
C2—C3—H3	120.1	N2—C18—C13	122.5 (4)
C4—C3—H3	120.1	C17—C18—C13	122.3 (4)
C9—C4—C5	117.4 (3)	Cl2—C19—Cl1	111.1 (2)
C9—C4—C3	116.6 (3)	Cl2—C19—H19A	109.4
C5—C4—C3	126.0 (3)	Cl1—C19—H19A	109.4
C6—C5—C4	119.8 (3)	Cl2—C19—H19B	109.4
C6—C5—H5	120.1	Cl1—C19—H19B	109.4
C4—C5—H5	120.1	H19A—C19—H19B	108.0
C5—C6—C7	122.5 (3)
O1—Ta1—O2—C8	74.2 (2)	C5—C6—C7—C8	−0.1 (5)
O2^i—Ta1—O2—C8	174.44 (19)	Ta1—O2—C8—C7	−173.5 (2)
O3—Ta1—O2—C8	−43.6 (3)	Ta1—O2—C8—C9	7.5 (4)
N1^i—Ta1—O2—C8	179.4 (2)	C6—C7—C8—O2	179.4 (3)
N1—Ta1—O2—C8	−8.7 (2)	C6—C7—C8—C9	−1.7 (4)
N2—Ta1—O2—C8	−100.0 (2)	C1—N1—C9—C4	−1.4 (4)
O1—Ta1—O3—C17	180.0	Ta1—N1—C9—C4	172.5 (2)
O2—Ta1—O3—C17	−60.13 (11)	C1—N1—C9—C8	178.5 (3)
O2^i—Ta1—O3—C17	60.13 (11)	Ta1—N1—C9—C8	−7.7 (3)
N1^i—Ta1—O3—C17	94.69 (7)	C5—C4—C9—N1	179.0 (3)
N1—Ta1—O3—C17	−94.69 (7)	C3—C4—C9—N1	1.0 (4)
N2—Ta1—O3—C17	0.0	C5—C4—C9—C8	−0.8 (4)
O1—Ta1—N1—C1	76.2 (3)	C3—C4—C9—C8	−178.8 (3)
O2—Ta1—N1—C1	−178.6 (3)	O2—C8—C9—N1	1.3 (4)
O2^i—Ta1—N1—C1	−173.6 (2)	C7—C8—C9—N1	−177.6 (3)
O3—Ta1—N1—C1	−22.6 (2)	O2—C8—C9—C4	−178.8 (3)
N1^i—Ta1—N1—C1	−6.9 (4)	C7—C8—C9—C4	2.2 (4)
N2—Ta1—N1—C1	−94.7 (3)	C18—N2—C10—C11	0.0
O1—Ta1—N1—C9	−96.8 (2)	Ta1—N2—C10—C11	180.0
O2—Ta1—N1—C9	8.44 (18)	N2—C10—C11—C12	0.0
O2^i—Ta1—N1—C9	13.4 (3)	C10—C11—C12—C13	0.0
O3—Ta1—N1—C9	164.4 (2)	C11—C12—C13—C18	0.0
N1^i—Ta1—N1—C9	−179.87 (13)	C11—C12—C13—C14	180.0
N2—Ta1—N1—C9	92.3 (2)	C12—C13—C14—C15	180.0
O2—Ta1—N2—C10	−36.35 (6)	C18—C13—C14—C15	0.0
O2^i—Ta1—N2—C10	36.35 (6)	C13—C14—C15—C16	0.0
O3—Ta1—N2—C10	180.0	C14—C15—C16—C17	0.0
N1^i—Ta1—N2—C10	107.56 (7)	Ta1—O3—C17—C16	180.0
N1—Ta1—N2—C10	−107.56 (7)	Ta1—O3—C17—C18	0.0
O2—Ta1—N2—C18	143.65 (6)	C15—C16—C17—O3	180.0
O2^i—Ta1—N2—C18	−143.65 (6)	C15—C16—C17—C18	0.0
O3—Ta1—N2—C18	0.0	C10—N2—C18—C17	180.0
N1^i—Ta1—N2—C18	−72.44 (7)	Ta1—N2—C18—C17	0.0
N1—Ta1—N2—C18	72.44 (7)	C10—N2—C18—C13	0.0
C9—N1—C1—C2	0.4 (4)	Ta1—N2—C18—C13	180.0
Ta1—N1—C1—C2	−172.3 (2)	O3—C17—C18—N2	0.0
N1—C1—C2—C3	0.8 (5)	C16—C17—C18—N2	180.0
C1—C2—C3—C4	−1.1 (4)	O3—C17—C18—C13	180.0
C2—C3—C4—C9	0.2 (4)	C16—C17—C18—C13	0.0
C2—C3—C4—C5	−177.5 (3)	C12—C13—C18—N2	0.0
C9—C4—C5—C6	−1.0 (4)	C14—C13—C18—N2	180.0
C3—C4—C5—C6	176.7 (3)	C12—C13—C18—C17	180.0
C4—C5—C6—C7	1.5 (5)	C14—C13—C18—C17	0.0

Symmetry code: (i) x, −y+1/2, z.