fac-Tri­aqua­[tris(2-pyridyl)­amine-κ³N]­chromium(III) tris­(tri­fluoro­methane­sulfonate)

In the title compound, fac-[Cr(tpa)(H₂O)₃](CF₃SO₃)₃ [tpa is tris(2-pyridyl)­amine; C₁₅H₁₂N₄], the Cr^III ion is coordinated by the symmetry-related N atoms of tpa, which acts as a tripodal ligand, and O atoms of water; a threefold rotation axis passes through the Cr and amine N atoms, with Cr—N_pyridyl and Cr—O distances of 2.0403 (12) and 1.9815 (11) Å, respectively. A three-dimensional network is formed by intermolecular O—H...O hydrogen bonds between coordinated water mol­ecules and sulfonate groups of the anions.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](C-C) = 0.002 Å
• R factor = 0.032
• wR factor = 0.089
• Data-to-parameter ratio = 17.1

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT244_ALERT_4_C Low Solvent  U(eq) as Compared to Neighbors ....         S2
PLAT244_ALERT_4_C Low Solvent  U(eq) as Compared to Neighbors ....         C6
PLAT354_ALERT_3_C Short   O-H Bond (0.82A)   O1     -   H10    ...       0.71 Ang.

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   4 ALERT level C = Check and explain
   0 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
   1 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: SMART-W2K/NT (Bruker, 2003); cell refinement: SMART-W2K/NT; data reduction: SAINT-W2K/NT (Bruker, 2003); program(s) used to solve structure: SHELXTL-NT (Bruker, 2003); program(s) used to refine structure: SHELXTL-NT; molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXTL-NT.

fac-Triaqua[tris(2-pyridyl)amine]chromium(III) trifluoromethanesulfonate

Crystal data

[Cr(C15H12N4)(H2O)3](CF3SO3)3	Dx = 1.721 Mg m^−3
Mr = 801.54	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P3	Cell parameters from 8816 reflections
Hall symbol: -P 3	θ = 2.7–28.3°
a = 13.0562 (3) Å	µ = 0.69 mm^−1
c = 10.4754 (5) Å	T = 173 K
V = 1546.45 (9) Å^3	Block, red
Z = 2	0.52 × 0.51 × 0.32 mm
F(000) = 806

Data collection

Bruker SMART APEX CCD area-detector diffractometer	2563 independent reflections
Radiation source: fine-focus sealed tube	2413 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.044
Detector resolution: 8.366 pixels mm^-1	θmax = 28.3°, θmin = 1.8°
φ and ω scans	h = −11→17
Absorption correction: multi-scan (SADABS; Scheldrick, 1996)	k = −17→13
Tmin = 0.716, Tmax = 0.810	l = −13→13
11598 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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.089	H atoms treated by a mixture of independent and constrained refinement
S = 1.07	w = 1/[σ^2(Fo^2) + (0.0476P)^2 + 0.7758P] where P = (Fo^2 + 2Fc^2)/3
2563 reflections	(Δ/σ)max = 0.001
150 parameters	Δρmax = 0.35 e Å^−3
0 restraints	Δρmin = −0.47 e Å^−3

Special details

Experimental. none

Geometry. Angle with sdev

52.10(0.03) N1—Cr1—N2

Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane)

10.8598 (0.0048) x + 0.8404 (0.0085) y - 0.2617 (0.0070) z = 7.3043 (0.0059)

* 0.0020 (0.0009) N1 * -0.0048 (0.0010) C1 * 0.0026 (0.0011) C2 * 0.0022 (0.0012) C3 * -0.0049 (0.0012) C4 * 0.0029 (0.0011) C5

Rms deviation of fitted atoms = 0.0034

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
Cr1	0.6667	0.3333	0.61522 (3)	0.01738 (11)
N1	0.65562 (10)	0.45075 (10)	0.73486 (11)	0.0205 (2)
N2	0.6667	0.3333	0.90160 (19)	0.0209 (4)
O1	0.78024 (10)	0.46132 (10)	0.50174 (11)	0.0244 (2)
C1	0.65926 (12)	0.43497 (12)	0.86158 (13)	0.0211 (3)
C2	0.65618 (14)	0.51100 (14)	0.95036 (14)	0.0285 (3)
C3	0.64762 (16)	0.60705 (15)	0.90668 (16)	0.0339 (3)
C4	0.64271 (16)	0.62306 (14)	0.77688 (17)	0.0323 (3)
C5	0.64748 (13)	0.54401 (13)	0.69335 (14)	0.0261 (3)
H2	0.6598	0.4982	1.0391	0.034*
H3	0.6452	0.6612	0.9655	0.041*
H4	0.6361	0.6878	0.7456	0.039*
H5	0.6450	0.5556	0.6041	0.031*
H10	0.836 (3)	0.506 (2)	0.524 (3)	0.051 (8)*
H11	0.759 (2)	0.483 (2)	0.442 (2)	0.040 (6)*
C6	0.81468 (19)	0.78434 (19)	0.2965 (3)	0.0517 (5)
F1	0.87054 (13)	0.79432 (16)	0.18730 (17)	0.0768 (5)
F2	0.88681 (13)	0.79619 (17)	0.39179 (19)	0.0835 (5)
F3	0.78838 (17)	0.86921 (13)	0.3048 (3)	0.0997 (7)
S2	0.68084 (3)	0.64109 (3)	0.30528 (3)	0.02578 (11)
O2	0.63078 (12)	0.64370 (15)	0.42784 (12)	0.0442 (3)
O3	0.72438 (12)	0.55845 (11)	0.30167 (12)	0.0378 (3)
O4	0.61319 (11)	0.63906 (13)	0.19726 (11)	0.0390 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.01827 (13)	0.01827 (13)	0.01560 (18)	0.00914 (7)	0.000	0.000
N1	0.0215 (5)	0.0201 (5)	0.0200 (5)	0.0106 (4)	0.0008 (4)	−0.0002 (4)
N2	0.0215 (6)	0.0215 (6)	0.0198 (9)	0.0108 (3)	0.000	0.000
O1	0.0223 (5)	0.0241 (5)	0.0220 (5)	0.0080 (4)	0.0000 (4)	0.0034 (4)
C1	0.0201 (6)	0.0211 (6)	0.0215 (6)	0.0097 (5)	0.0007 (5)	−0.0004 (5)
C2	0.0335 (7)	0.0283 (7)	0.0235 (7)	0.0155 (6)	0.0010 (5)	−0.0039 (5)
C3	0.0436 (9)	0.0283 (7)	0.0337 (8)	0.0210 (7)	0.0016 (7)	−0.0072 (6)
C4	0.0400 (8)	0.0244 (7)	0.0368 (8)	0.0194 (7)	0.0018 (7)	0.0004 (6)
C5	0.0303 (7)	0.0235 (6)	0.0261 (7)	0.0146 (6)	0.0012 (5)	0.0024 (5)
C6	0.0363 (9)	0.0365 (10)	0.0792 (15)	0.0161 (8)	−0.0052 (10)	−0.0017 (10)
F1	0.0454 (7)	0.0769 (10)	0.0957 (12)	0.0214 (7)	0.0281 (8)	0.0416 (9)
F2	0.0426 (8)	0.0868 (12)	0.1038 (13)	0.0194 (8)	−0.0329 (8)	−0.0285 (10)
F3	0.0803 (12)	0.0348 (7)	0.185 (2)	0.0294 (8)	−0.0098 (13)	−0.0089 (10)
S2	0.02477 (18)	0.0332 (2)	0.02258 (19)	0.01688 (15)	0.00129 (12)	0.00198 (13)
O2	0.0474 (8)	0.0816 (10)	0.0247 (6)	0.0480 (8)	0.0050 (5)	0.0057 (6)
O3	0.0471 (7)	0.0399 (7)	0.0372 (6)	0.0298 (6)	0.0073 (5)	0.0072 (5)
O4	0.0353 (6)	0.0563 (8)	0.0273 (6)	0.0242 (6)	−0.0041 (5)	0.0015 (5)

Geometric parameters (Å, º)

Cr1—O1^i	1.9815 (11)	N2—C1^i	1.4402 (15)
Cr1—O1^ii	1.9815 (11)	N2—C1^ii	1.4402 (15)
Cr1—O1	1.9815 (11)	N2—C1	1.4402 (15)
Cr1—N1^ii	2.0403 (12)	C1—C2	1.375 (2)
Cr1—N1^i	2.0403 (12)	C5—C4	1.378 (2)
Cr1—N1	2.0403 (12)	C5—H5	0.9500
S2—O4	1.4274 (12)	C2—C3	1.391 (2)
S2—O2	1.4487 (12)	C2—H2	0.9500
S2—O3	1.4500 (12)	C4—C3	1.382 (2)
S2—C6	1.814 (2)	C4—H4	0.9500
O1—H10	0.71 (3)	C3—H3	0.9500
O1—H11	0.79 (3)	F1—C6	1.327 (3)
N1—C5	1.3461 (18)	F2—C6	1.328 (3)
N1—C1	1.3478 (18)	F3—C6	1.317 (3)
O1^i—Cr1—O1^ii	87.71 (5)	C1—N1—Cr1	117.96 (9)
O1^i—Cr1—O1	87.71 (5)	C1^i—N2—C1^ii	111.90 (8)
O1^ii—Cr1—O1	87.71 (5)	C1^i—N2—C1	111.90 (8)
O1^i—Cr1—N1^ii	178.45 (5)	C1^ii—N2—C1	111.89 (8)
O1^ii—Cr1—N1^ii	92.24 (5)	N1—C1—C2	122.65 (13)
O1—Cr1—N1^ii	93.83 (5)	N1—C1—N2	116.83 (13)
O1^i—Cr1—N1^i	92.24 (5)	C2—C1—N2	120.52 (14)
O1^ii—Cr1—N1^i	93.83 (5)	N1—C5—C4	121.73 (14)
O1—Cr1—N1^i	178.45 (5)	N1—C5—H5	119.1
N1^ii—Cr1—N1^i	86.22 (5)	C4—C5—H5	119.1
O1^i—Cr1—N1	93.83 (5)	C1—C2—C3	118.22 (14)
O1^ii—Cr1—N1	178.45 (5)	C1—C2—H2	120.9
O1—Cr1—N1	92.24 (5)	C3—C2—H2	120.9
N1^ii—Cr1—N1	86.22 (5)	C5—C4—C3	119.25 (14)
N1^i—Cr1—N1	86.22 (5)	C5—C4—H4	120.4
O4—S2—O2	114.88 (8)	C3—C4—H4	120.4
O4—S2—O3	115.76 (8)	C4—C3—C2	119.38 (14)
O2—S2—O3	112.95 (8)	C4—C3—H3	120.3
O4—S2—C6	104.29 (10)	C2—C3—H3	120.3
O2—S2—C6	103.54 (11)	F3—C6—F1	109.6 (2)
O3—S2—C6	103.41 (9)	F3—C6—F2	108.7 (2)
Cr1—O1—H10	122 (2)	F1—C6—F2	108.29 (19)
Cr1—O1—H11	122.1 (17)	F3—C6—S2	110.00 (16)
H10—O1—H11	111 (3)	F1—C6—S2	110.11 (16)
C5—N1—C1	118.77 (12)	F2—C6—S2	110.08 (17)
C5—N1—Cr1	123.26 (10)
O1^i—Cr1—N1—C5	−45.13 (12)	C1—N1—C5—C4	−0.1 (2)
O1—Cr1—N1—C5	42.73 (12)	Cr1—N1—C5—C4	−178.59 (12)
N1^ii—Cr1—N1—C5	136.42 (13)	N1—C1—C2—C3	0.7 (2)
N1^i—Cr1—N1—C5	−137.12 (13)	N2—C1—C2—C3	−179.26 (13)
O1^i—Cr1—N1—C1	136.34 (10)	N1—C5—C4—C3	0.7 (3)
O1—Cr1—N1—C1	−135.80 (10)	C5—C4—C3—C2	−0.6 (3)
N1^ii—Cr1—N1—C1	−42.11 (8)	C1—C2—C3—C4	−0.1 (3)
N1^i—Cr1—N1—C1	44.35 (8)	O4—S2—C6—F3	61.4 (2)
C5—N1—C1—C2	−0.7 (2)	O2—S2—C6—F3	−59.1 (2)
Cr1—N1—C1—C2	177.94 (11)	O3—S2—C6—F3	−177.11 (19)
C5—N1—C1—N2	179.34 (11)	O4—S2—C6—F1	−59.52 (17)
Cr1—N1—C1—N2	−2.06 (15)	O2—S2—C6—F1	179.95 (14)
C1^i—N2—C1—N1	−61.95 (16)	O3—S2—C6—F1	61.94 (17)
C1^ii—N2—C1—N1	64.54 (15)	O4—S2—C6—F2	−178.84 (16)
C1^i—N2—C1—C2	118.05 (18)	O2—S2—C6—F2	60.64 (18)
C1^ii—N2—C1—C2	−115.46 (18)	O3—S2—C6—F2	−57.38 (18)

Symmetry codes: (i) −y+1, x−y, z; (ii) −x+y+1, −x+1, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H10···O2^iii	0.71 (3)	1.89 (3)	2.5995 (17)	176 (3)
O1—H11···O3	0.79 (3)	1.94 (3)	2.7308 (17)	172 (2)

Symmetry code: (iii) x−y+1, x, −z+1.