μ-Oxido-bis-{chlorido[tris-(2-pyridylmeth-yl)amine]chromium(III)} bis(hexafluoridophosphate).

The title compound, [Cr(2)Cl(2)O(C(18)H(18)N(4))(2)](PF(6))(2), is isostructural with the V(III) analogue. Each Cr(III) atom is chelated by the tetra-dentate tris-(2-pyridylmeth-yl)amine ligand via four N atoms, and further coordinated by one Cl atom and one bridging O atom, giving a slightly distorted octa-hedral coordination geometry. The dinuclear complex is centrosymmetric, with the bridging O atom lying on a centre of inversion.

Related literature

For the isostructural VIII analogue, see: Tajika et al. (2005 ▶). For more general related literature, see: Butler & Carrano (1991 ▶); Crans et al. (1989 ▶); Dey (1974 ▶); Chen & Zubieta (1990 ▶).

Experimental

Crystal data

[Cr2Cl2O(C18H18N4)2](PF6)2

M = 1061.57

Triclinic,

a = 8.6107 (17) Å

b = 11.302 (2) Å

c = 12.798 (3) Å

α = 115.50 (3)°

β = 107.45 (3)°

γ = 91.50 (3)°

V = 1054.8 (4) Å3

Z = 1

Mo Kα radiation

μ = 0.81 mm−1

T = 293 (2) K

0.28 × 0.22 × 0.18 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.804, T max = 0.867

8686 measured reflections

3877 independent reflections

3594 reflections with I > 2σ(I)

R int = 0.021

Refinement

R[F 2 > 2σ(F 2)] = 0.033

wR(F 2) = 0.089

S = 1.00

3877 reflections

287 parameters

H-atom parameters constrained

Δρmax = 0.51 e Å−3

Δρmin = −0.33 e Å−3

Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT-Plus (Bruker, 2001 ▶); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997 ▶); molecular graphics: SHELXTL (Bruker, 2001 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536807061296/bi2257sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536807061296/bi2257Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Cr2Cl2O(C18H18N4)2](PF6)2	Z = 1
Mr = 1061.57	F000 = 536
Triclinic, P1	Dx = 1.671 Mg m−3
Hall symbol: -P 1	Mo Kα radiation λ = 0.71073 Å
a = 8.6107 (17) Å	Cell parameters from 3877 reflections
b = 11.302 (2) Å	θ = 3.0–25.5º
c = 12.798 (3) Å	µ = 0.81 mm−1
α = 115.50 (3)º	T = 293 (2) K
β = 107.45 (3)º	Block, blue
γ = 91.50 (3)º	0.28 × 0.22 × 0.18 mm
V = 1054.8 (4) Å3

Bruker APEX II CCD diffractometer	3877 independent reflections
Radiation source: fine-focus sealed tube	3594 reflections with I > 2σ(I)
Monochromator: graphite	Rint = 0.021
T = 293(2) K	θmax = 25.5º
φ and ω scans	θmin = 3.0º
Absorption correction: multi-scan(SADABS; Bruker, 2001)	h = −8→10
Tmin = 0.804, Tmax = 0.867	k = −13→13
8686 measured reflections	l = −15→15

Refinement on F2	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F2 > 2σ(F2)] = 0.033	w = 1/[σ2(Fo2) + (0.0565P)2 + 0.3428P] where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.089	(Δ/σ)max < 0.001
S = 1.00	Δρmax = 0.51 e Å−3
3877 reflections	Δρmin = −0.33 e Å−3
287 parameters	Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.042 (3)
Secondary atom site location: difference Fourier map

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
Cr1	1.03745 (3)	0.34679 (3)	0.39271 (2)	0.0408 (4)
C1	0.9871 (3)	0.1897 (2)	0.53070 (18)	0.0447 (4)
H1	1.1018	0.1984	0.5573	0.054*
C2	0.8992 (3)	0.1306 (2)	0.5741 (2)	0.0534 (5)
H2	0.9533	0.0998	0.6296	0.064*
C3	0.7284 (3)	0.1173 (3)	0.5340 (2)	0.0605 (6)
H3	0.6662	0.0779	0.5626	0.073*
C4	0.6514 (3)	0.1630 (2)	0.4513 (2)	0.0552 (5)
H4	0.5367	0.1537	0.4226	0.066*
C5	0.7464 (2)	0.22306 (19)	0.41135 (18)	0.0425 (4)
C6	0.6721 (2)	0.2874 (2)	0.3310 (2)	0.0490 (5)
H6A	0.5643	0.2353	0.2730	0.059*
H6B	0.6563	0.3757	0.3822	0.059*
C7	0.7467 (3)	0.1753 (2)	0.1450 (2)	0.0573 (6)
H7A	0.7443	0.2004	0.0811	0.069*
H7B	0.6381	0.1253	0.1216	0.069*
C8	0.8712 (2)	0.08565 (19)	0.14924 (17)	0.0414 (4)
C9	0.8351 (3)	−0.0448 (2)	0.0588 (2)	0.0528 (5)
H9	0.7315	−0.0793	−0.0028	0.063*
C10	0.9546 (3)	−0.1237 (2)	0.0606 (2)	0.0617 (6)
H10	0.9327	−0.2119	0.0003	0.074*
C11	1.1069 (3)	−0.0697 (2)	0.1532 (2)	0.0607 (6)
H11	1.1894	−0.1208	0.1564	0.073*
C12	1.1346 (3)	0.0605 (2)	0.2404 (2)	0.0526 (5)
H12	1.2374	0.0964	0.3028	0.063*
C13	0.7605 (3)	0.4147 (2)	0.23723 (19)	0.0475 (5)
H13A	0.7430	0.4881	0.3059	0.057*
H13B	0.6651	0.3917	0.1639	0.057*
C14	0.9146 (3)	0.4574 (2)	0.21891 (17)	0.0471 (5)
C15	0.9138 (4)	0.5296 (2)	0.1547 (2)	0.0606 (6)
H15	0.8154	0.5482	0.1149	0.073*
C16	1.0629 (4)	0.5734 (3)	0.1512 (2)	0.0728 (8)
H16	1.0650	0.6237	0.1100	0.087*
C17	1.2075 (4)	0.5435 (3)	0.2077 (3)	0.0715 (7)
H17	1.3076	0.5721	0.2047	0.086*
C18	1.2007 (3)	0.4704 (3)	0.2686 (2)	0.0610 (6)
H18	1.2978	0.4490	0.3069	0.073*
Cl1	1.31398 (6)	0.35078 (6)	0.48445 (5)	0.05507 (17)
F1	0.5115 (2)	0.90789 (16)	0.13882 (17)	0.0825 (5)
F2	0.4878 (2)	0.8490 (2)	0.27945 (15)	0.0893 (5)
F3	0.5830 (3)	0.6607 (2)	0.1912 (2)	0.1078 (7)
F4	0.7325 (2)	0.8610 (2)	0.24906 (17)	0.0999 (6)
F5	0.6040 (2)	0.72005 (19)	0.04870 (17)	0.0929 (6)
F6	0.36012 (19)	0.71102 (16)	0.08031 (14)	0.0726 (4)
N1	1.0192 (2)	0.13917 (16)	0.23969 (15)	0.0436 (4)
N2	1.0566 (2)	0.42848 (18)	0.27454 (16)	0.0482 (4)
N3	0.91312 (19)	0.23567 (15)	0.45104 (15)	0.0406 (3)
N4	0.7776 (2)	0.29834 (16)	0.26214 (15)	0.0424 (4)
O1	1.0000	0.5000	0.5000	0.0420 (4)
P1	0.54870 (7)	0.78424 (6)	0.16549 (5)	0.05276 (17)

	U11	U22	U33	U12	U13	U23
Cr1	0.0378 (11)	0.0424 (10)	0.0424 (10)	0.0088 (8)	0.0112 (8)	0.0212 (8)
C1	0.0415 (10)	0.0468 (10)	0.0459 (10)	0.0095 (8)	0.0121 (8)	0.0233 (8)
C2	0.0597 (14)	0.0546 (12)	0.0513 (12)	0.0109 (10)	0.0179 (10)	0.0300 (10)
C3	0.0606 (14)	0.0666 (14)	0.0669 (14)	0.0057 (11)	0.0281 (11)	0.0381 (12)
C4	0.0395 (11)	0.0606 (13)	0.0695 (14)	0.0063 (9)	0.0206 (10)	0.0324 (11)
C5	0.0351 (9)	0.0412 (9)	0.0456 (10)	0.0057 (7)	0.0117 (8)	0.0166 (8)
C6	0.0302 (9)	0.0572 (12)	0.0614 (12)	0.0093 (8)	0.0107 (8)	0.0322 (10)
C7	0.0517 (13)	0.0499 (12)	0.0462 (11)	0.0099 (9)	−0.0011 (9)	0.0127 (9)
C8	0.0424 (10)	0.0438 (10)	0.0403 (9)	0.0052 (8)	0.0153 (8)	0.0207 (8)
C9	0.0562 (13)	0.0484 (11)	0.0497 (11)	0.0027 (9)	0.0185 (10)	0.0189 (9)
C10	0.0769 (17)	0.0441 (11)	0.0634 (14)	0.0138 (11)	0.0334 (13)	0.0178 (10)
C11	0.0653 (15)	0.0551 (13)	0.0714 (15)	0.0256 (11)	0.0342 (12)	0.0297 (11)
C12	0.0460 (12)	0.0572 (12)	0.0570 (12)	0.0167 (9)	0.0199 (10)	0.0265 (10)
C13	0.0504 (11)	0.0490 (11)	0.0410 (10)	0.0162 (9)	0.0097 (8)	0.0224 (9)
C14	0.0599 (13)	0.0426 (10)	0.0358 (9)	0.0112 (9)	0.0152 (9)	0.0162 (8)
C15	0.0864 (18)	0.0503 (12)	0.0451 (12)	0.0140 (11)	0.0197 (11)	0.0237 (10)
C16	0.114 (2)	0.0544 (13)	0.0572 (14)	0.0012 (14)	0.0362 (15)	0.0288 (12)
C17	0.084 (2)	0.0710 (16)	0.0683 (16)	−0.0005 (14)	0.0357 (14)	0.0343 (13)
C18	0.0612 (14)	0.0666 (14)	0.0615 (14)	0.0042 (11)	0.0280 (11)	0.0307 (12)
Cl1	0.0334 (3)	0.0609 (3)	0.0596 (3)	0.0131 (2)	0.0101 (2)	0.0215 (2)
F1	0.0810 (11)	0.0724 (10)	0.0988 (12)	0.0060 (8)	0.0208 (9)	0.0507 (9)
F2	0.0836 (12)	0.1141 (14)	0.0632 (9)	0.0059 (10)	0.0336 (8)	0.0300 (9)
F3	0.1008 (15)	0.1236 (16)	0.163 (2)	0.0524 (12)	0.0641 (14)	0.1074 (16)
F4	0.0483 (9)	0.1549 (19)	0.0854 (12)	−0.0063 (10)	0.0024 (8)	0.0605 (12)
F5	0.0973 (13)	0.0965 (12)	0.0873 (12)	0.0083 (10)	0.0563 (10)	0.0288 (10)
F6	0.0571 (9)	0.0710 (9)	0.0731 (9)	−0.0042 (7)	0.0144 (7)	0.0248 (7)
N1	0.0425 (9)	0.0456 (9)	0.0444 (9)	0.0116 (7)	0.0164 (7)	0.0210 (7)
N2	0.0526 (10)	0.0497 (9)	0.0451 (9)	0.0087 (8)	0.0187 (8)	0.0231 (8)
N3	0.0348 (8)	0.0421 (8)	0.0447 (8)	0.0082 (6)	0.0125 (7)	0.0205 (7)
N4	0.0376 (8)	0.0442 (8)	0.0411 (8)	0.0101 (7)	0.0077 (6)	0.0195 (7)
O1	0.0384 (10)	0.0430 (10)	0.0424 (10)	0.0081 (8)	0.0119 (8)	0.0190 (8)
P1	0.0429 (3)	0.0665 (4)	0.0529 (3)	0.0075 (3)	0.0151 (2)	0.0321 (3)

Cr1—O1	1.7986 (7)	C9—H9	0.930
Cr1—N3	2.1206 (18)	C10—C11	1.378 (4)
Cr1—N2	2.1238 (18)	C10—H10	0.930
Cr1—N4	2.2370 (19)	C11—C12	1.370 (3)
Cr1—N1	2.2814 (19)	C11—H11	0.930
Cr1—Cl1	2.3070 (9)	C12—N1	1.351 (3)
O1—Cr1i	1.7986 (7)	C12—H12	0.930
C1—N3	1.341 (3)	C13—N4	1.482 (3)
C1—C2	1.369 (3)	C13—C14	1.516 (3)
C1—H1	0.930	C13—H13A	0.970
C2—C3	1.386 (4)	C13—H13B	0.970
C2—H2	0.930	C14—N2	1.345 (3)
C3—C4	1.376 (4)	C14—C15	1.383 (3)
C3—H3	0.930	C15—C16	1.384 (4)
C4—C5	1.382 (3)	C15—H15	0.930
C4—H4	0.930	C16—C17	1.371 (4)
C5—N3	1.352 (3)	C16—H16	0.930
C5—C6	1.506 (3)	C17—C18	1.369 (4)
C6—N4	1.479 (3)	C17—H17	0.930
C6—H6A	0.970	C18—N2	1.351 (3)
C6—H6B	0.970	C18—H18	0.930
C7—N4	1.483 (3)	F1—P1	1.5939 (17)
C7—C8	1.499 (3)	F2—P1	1.5803 (18)
C7—H7A	0.970	F3—P1	1.582 (2)
C7—H7B	0.970	F4—P1	1.5859 (18)
C8—N1	1.342 (3)	F5—P1	1.5804 (18)
C8—C9	1.379 (3)	F6—P1	1.6129 (17)
C9—C10	1.380 (4)
O1—Cr1—N3	91.01 (5)	N1—C12—H12	118.5
O1—Cr1—N2	92.46 (5)	C11—C12—H12	118.5
N3—Cr1—N2	154.67 (7)	N4—C13—C14	110.48 (16)
O1—Cr1—N4	91.36 (6)	N4—C13—H13A	109.6
N3—Cr1—N4	78.03 (7)	C14—C13—H13A	109.6
N2—Cr1—N4	76.81 (7)	N4—C13—H13B	109.6
O1—Cr1—N1	166.58 (5)	C14—C13—H13B	109.6
N3—Cr1—N1	81.87 (7)	H13A—C13—H13B	108.1
N2—Cr1—N1	89.30 (7)	N2—C14—C15	120.7 (2)
N4—Cr1—N1	76.09 (7)	N2—C14—C13	116.67 (18)
O1—Cr1—Cl1	103.29 (5)	C15—C14—C13	122.5 (2)
N3—Cr1—Cl1	104.03 (5)	C14—C15—C16	118.4 (3)
N2—Cr1—Cl1	99.56 (6)	C14—C15—H15	120.8
N4—Cr1—Cl1	165.11 (5)	C16—C15—H15	120.8
N1—Cr1—Cl1	89.52 (6)	C17—C16—C15	120.8 (2)
N3—C1—C2	122.1 (2)	C17—C16—H16	119.6
N3—C1—H1	118.9	C15—C16—H16	119.6
C2—C1—H1	119.0	C16—C17—C18	118.2 (3)
C3—C2—C1	118.8 (2)	C16—C17—H17	120.9
C3—C2—H2	120.6	C18—C17—H17	120.9
C1—C2—H2	120.6	N2—C18—C17	121.8 (3)
C2—C3—C4	119.4 (2)	N2—C18—H18	119.1
C2—C3—H3	120.3	C17—C18—H18	119.1
C4—C3—H3	120.3	C12—N1—C8	117.79 (18)
C3—C4—C5	119.3 (2)	C12—N1—Cr1	126.02 (15)
C3—C4—H4	120.4	C8—N1—Cr1	115.61 (13)
C5—C4—H4	120.4	C14—N2—C18	120.1 (2)
N3—C5—C4	120.95 (19)	C14—N2—Cr1	114.45 (14)
N3—C5—C6	116.79 (18)	C18—N2—Cr1	124.62 (17)
C4—C5—C6	122.07 (19)	C1—N3—C5	119.42 (18)
N4—C6—C5	112.19 (16)	C1—N3—Cr1	125.22 (14)
N4—C6—H6A	109.2	C5—N3—Cr1	115.07 (13)
C5—C6—H6A	109.2	C6—N4—C7	112.30 (18)
N4—C6—H6B	109.2	C6—N4—C13	112.63 (16)
C5—C6—H6B	109.2	C7—N4—C13	109.74 (17)
H6A—C6—H6B	107.9	C6—N4—Cr1	105.11 (12)
N4—C7—C8	114.97 (17)	C7—N4—Cr1	112.78 (13)
N4—C7—H7A	108.5	C13—N4—Cr1	103.96 (12)
C8—C7—H7A	108.5	Cr1—O1—Cr1i	180.0
N4—C7—H7B	108.5	F5—P1—F3	90.59 (12)
C8—C7—H7B	108.5	F5—P1—F2	178.06 (11)
H7A—C7—H7B	107.5	F3—P1—F2	90.59 (13)
N1—C8—C9	122.2 (2)	F5—P1—F4	90.15 (11)
N1—C8—C7	117.57 (17)	F3—P1—F4	91.62 (13)
C9—C8—C7	120.13 (19)	F2—P1—F4	91.35 (11)
C10—C9—C8	119.3 (2)	F5—P1—F1	89.58 (11)
C10—C9—H9	120.4	F3—P1—F1	179.22 (11)
C8—C9—H9	120.4	F2—P1—F1	89.22 (11)
C11—C10—C9	118.9 (2)	F4—P1—F1	89.14 (11)
C11—C10—H10	120.5	F5—P1—F6	90.19 (10)
C9—C10—H10	120.5	F3—P1—F6	90.39 (12)
C10—C11—C12	118.9 (2)	F2—P1—F6	88.26 (10)
C10—C11—H11	120.6	F4—P1—F6	177.95 (11)
C12—C11—H11	120.6	F1—P1—F6	88.85 (10)
N1—C12—C11	122.9 (2)