Aqua-(2,2'-bipyridine)trifluorido-chromium(III) dihydrate.

The title compound, [CrF(3)(C(10)H(8)N(2))(H(2)O)]·2H(2)O, was prepared by the reaction of CrF(3) and 2,2'-bipyridine under hydrous conditions. The metal centre is coordinated in a distorted octahedral mode by two N atoms from the organic ligand, three F atoms and one O atom of a water molecule. . The crystal packing is stabilized by O-H⋯O and O-H⋯F hydrogen-bonding contacts, which form a one-dimensional belt extending parallel to (100).

Related literature

For anion structures, see: Kumar et al. (2007 ▶); Krishnan et al. (2007 ▶); Wu et al. (2007 ▶); Dong et al. (2005 ▶). For related structures, see: Timco et al. (2005 ▶); Larsen et al. (2003 ▶); Ochsenbein et al. (2008 ▶).

Experimental

Crystal data

[CrF3(C10H8N2)(H2O)]·2H2O

M = 319.23

Monoclinic,

a = 9.0100 (18) Å

b = 7.4170 (15) Å

c = 20.759 (6) Å

β = 112.35 (3)°

V = 1283.1 (5) Å3

Z = 4

Mo Kα radiation

μ = 0.93 mm−1

T = 293 K

0.24 × 0.18 × 0.17 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: none

6478 measured reflections

2257 independent reflections

1916 reflections with I > 2σ(I)

R int = 0.023

Refinement

R[F 2 > 2σ(F 2)] = 0.040

wR(F 2) = 0.129

S = 1.12

2257 reflections

175 parameters

3 restraints

H-atom parameters constrained

Δρmax = 0.52 e Å−3

Δρmin = −0.56 e Å−3

Data collection: SMART (Bruker, 1997 ▶); cell refinement: SAINT (Bruker, 1997 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXTL.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809031808/br2114sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809031808/br2114Isup2.hkl

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

[CrF3(C10H8N2)(H2O)]·2H2O	F(000) = 652
Mr = 319.23	Dx = 1.653 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 1024 reflections
a = 9.0100 (18) Å	θ = 2.4–25.0°
b = 7.4170 (15) Å	µ = 0.93 mm−1
c = 20.759 (6) Å	T = 293 K
β = 112.35 (3)°	Prism, brown
V = 1283.1 (5) Å3	0.24 × 0.18 × 0.17 mm
Z = 4

Bruker SMART CCD area-detector diffractometer	1916 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.023
graphite	θmax = 25.0°, θmin = 2.4°
φ and ω scans	h = −10→10
6478 measured reflections	k = −8→8
2257 independent reflections	l = −21→24

Refinement on F2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.129	H-atom parameters constrained
S = 1.12	w = 1/[σ2(Fo2) + (0.0755P)2 + 0.6391P] where P = (Fo2 + 2Fc2)/3
2257 reflections	(Δ/σ)max < 0.001
175 parameters	Δρmax = 0.52 e Å−3
3 restraints	Δρmin = −0.56 e Å−3

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	0.15638 (5)	0.28271 (7)	0.32953 (2)	0.0283 (2)
F1	0.2014 (2)	0.0442 (2)	0.31271 (9)	0.0393 (5)
F2	0.1128 (2)	0.5267 (2)	0.34286 (9)	0.0436 (5)
F3	−0.0083 (2)	0.2083 (3)	0.35635 (12)	0.0521 (6)
N1	0.3615 (3)	0.3591 (4)	0.31451 (13)	0.0331 (6)
N2	0.3252 (3)	0.2663 (3)	0.42877 (13)	0.0318 (6)
C1	0.3689 (4)	0.4133 (5)	0.25417 (18)	0.0453 (8)
H1A	0.2741	0.4299	0.2157	0.054*
C2	0.5145 (5)	0.4453 (5)	0.2477 (2)	0.0540 (10)
H2A	0.5168	0.4829	0.2054	0.065*
C3	0.6529 (5)	0.4212 (6)	0.3035 (2)	0.0579 (10)
H3A	0.7513	0.4406	0.2997	0.069*
C4	0.6469 (4)	0.3678 (6)	0.3661 (2)	0.0533 (10)
H4A	0.7410	0.3513	0.4050	0.064*
C5	0.4997 (4)	0.3393 (4)	0.37029 (17)	0.0358 (7)
C6	0.4791 (4)	0.2890 (4)	0.43569 (17)	0.0353 (7)
C7	0.6048 (5)	0.2693 (5)	0.4996 (2)	0.0506 (10)
H7A	0.7105	0.2842	0.5037	0.061*
C8	0.5698 (6)	0.2272 (6)	0.5569 (2)	0.0613 (12)
H8A	0.6521	0.2127	0.6003	0.074*
C9	0.4128 (5)	0.2068 (5)	0.54970 (18)	0.0559 (11)
H9A	0.3875	0.1802	0.5881	0.067*
C10	0.2933 (5)	0.2264 (5)	0.48461 (18)	0.0432 (8)
H10A	0.1870	0.2113	0.4796	0.052*
O1W	0.0184 (3)	0.3056 (3)	0.22962 (11)	0.0363 (5)
H1W1	−0.0536	0.3443	0.1923	0.044*
H2W1	0.0476	0.2023	0.2211	0.044*
O2W	0.0891 (5)	0.4622 (5)	0.06932 (16)	0.0883 (11)
H1W2	0.0245	0.4742	0.0901	0.106*
H2W2	0.1487	0.3719	0.0871	0.106*
O3W	0.9992 (4)	0.1082 (5)	0.05359 (17)	0.0790 (10)
H2W3	0.9750	0.0764	0.0850	0.095*
H1W3	1.0333	0.0066	0.0477	0.095*

	U11	U22	U33	U12	U13	U23
Cr1	0.0252 (3)	0.0273 (3)	0.0288 (3)	0.00016 (18)	0.0059 (2)	0.00170 (18)
F1	0.0344 (10)	0.0296 (10)	0.0462 (10)	0.0000 (8)	0.0068 (8)	−0.0007 (8)
F2	0.0530 (12)	0.0329 (10)	0.0371 (10)	0.0091 (9)	0.0084 (9)	−0.0017 (8)
F3	0.0343 (11)	0.0647 (15)	0.0608 (13)	−0.0003 (10)	0.0221 (10)	0.0137 (10)
N1	0.0326 (14)	0.0322 (14)	0.0334 (14)	−0.0042 (11)	0.0113 (11)	0.0016 (11)
N2	0.0322 (14)	0.0298 (14)	0.0288 (14)	−0.0015 (11)	0.0063 (11)	0.0028 (10)
C1	0.048 (2)	0.046 (2)	0.0418 (19)	−0.0066 (17)	0.0172 (16)	0.0051 (15)
C2	0.068 (3)	0.050 (2)	0.059 (2)	−0.0085 (19)	0.042 (2)	0.0035 (18)
C3	0.043 (2)	0.066 (3)	0.072 (3)	−0.0106 (19)	0.030 (2)	−0.001 (2)
C4	0.0329 (18)	0.063 (2)	0.062 (2)	−0.0048 (18)	0.0159 (17)	0.000 (2)
C5	0.0315 (16)	0.0313 (16)	0.0425 (18)	−0.0038 (13)	0.0116 (14)	−0.0021 (14)
C6	0.0303 (17)	0.0296 (17)	0.0384 (18)	−0.0028 (13)	0.0046 (14)	−0.0014 (13)
C7	0.0354 (19)	0.052 (2)	0.046 (2)	−0.0042 (16)	−0.0048 (17)	0.0025 (16)
C8	0.062 (3)	0.062 (3)	0.037 (2)	−0.003 (2)	−0.0079 (19)	0.0087 (17)
C9	0.072 (3)	0.057 (3)	0.0294 (19)	−0.006 (2)	0.0090 (18)	0.0086 (16)
C10	0.045 (2)	0.045 (2)	0.0367 (19)	−0.0040 (16)	0.0128 (16)	0.0048 (15)
O1W	0.0351 (12)	0.0310 (11)	0.0305 (11)	0.0072 (9)	−0.0013 (9)	−0.0002 (9)
O2W	0.124 (3)	0.079 (2)	0.081 (2)	0.037 (2)	0.060 (2)	0.0043 (18)
O3W	0.096 (2)	0.083 (2)	0.079 (2)	−0.002 (2)	0.0559 (19)	0.0067 (19)

Cr1—F3	1.856 (2)	C4—H4A	0.9300
Cr1—F1	1.8769 (18)	C5—C6	1.486 (5)
Cr1—F2	1.8942 (19)	C6—C7	1.386 (5)
Cr1—O1W	1.979 (2)	C7—C8	1.379 (6)
Cr1—N2	2.047 (3)	C7—H7A	0.9300
Cr1—N1	2.067 (3)	C8—C9	1.373 (6)
N1—C1	1.341 (4)	C8—H8A	0.9300
N1—C5	1.348 (4)	C9—C10	1.378 (5)
N2—C10	1.329 (4)	C9—H9A	0.9300
N2—C6	1.350 (4)	C10—H10A	0.9300
C1—C2	1.388 (5)	O1W—H1W1	0.8498
C1—H1A	0.9300	O1W—H2W1	0.8500
C2—C3	1.353 (6)	O2W—H1W2	0.8500
C2—H2A	0.9300	O2W—H2W2	0.8500
C3—C4	1.378 (6)	O3W—H2W3	0.7978
C3—H3A	0.9300	O3W—H1W3	0.840 (10)
C4—C5	1.378 (5)
F3—Cr1—F1	91.69 (9)	C2—C3—H3A	120.3
F3—Cr1—F2	90.37 (10)	C4—C3—H3A	120.3
F1—Cr1—F2	177.37 (8)	C3—C4—C5	119.1 (4)
F3—Cr1—O1W	94.86 (10)	C3—C4—H4A	120.4
F1—Cr1—O1W	88.84 (8)	C5—C4—H4A	120.4
F2—Cr1—O1W	89.35 (8)	N1—C5—C4	121.7 (3)
F3—Cr1—N2	93.05 (10)	N1—C5—C6	114.7 (3)
F1—Cr1—N2	90.05 (9)	C4—C5—C6	123.6 (3)
F2—Cr1—N2	91.48 (9)	N2—C6—C7	121.4 (3)
O1W—Cr1—N2	172.04 (10)	N2—C6—C5	114.5 (3)
F3—Cr1—N1	171.69 (10)	C7—C6—C5	124.1 (3)
F1—Cr1—N1	87.80 (9)	C8—C7—C6	118.6 (4)
F2—Cr1—N1	90.39 (10)	C8—C7—H7A	120.7
O1W—Cr1—N1	93.42 (10)	C6—C7—H7A	120.7
N2—Cr1—N1	78.66 (11)	C9—C8—C7	119.7 (4)
C1—N1—C5	118.5 (3)	C9—C8—H8A	120.2
C1—N1—Cr1	126.0 (2)	C7—C8—H8A	120.2
C5—N1—Cr1	115.3 (2)	C8—C9—C10	118.9 (4)
C10—N2—C6	119.3 (3)	C8—C9—H9A	120.5
C10—N2—Cr1	124.5 (2)	C10—C9—H9A	120.5
C6—N2—Cr1	116.1 (2)	N2—C10—C9	122.1 (4)
N1—C1—C2	121.7 (3)	N2—C10—H10A	119.0
N1—C1—H1A	119.1	C9—C10—H10A	119.0
C2—C1—H1A	119.1	Cr1—O1W—H1W1	160.5
C3—C2—C1	119.5 (3)	Cr1—O1W—H2W1	91.2
C3—C2—H2A	120.3	H1W1—O1W—H2W1	107.7
C1—C2—H2A	120.3	H1W2—O2W—H2W2	107.7
C2—C3—C4	119.4 (4)	H2W3—O3W—H1W3	94.7

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H2W1···F1	0.85	2.22	2.699 (3)	116
O1W—H2W1···F2i	0.85	2.02	2.567 (3)	121
O1W—H2W1···F2i	0.85	2.02	2.567 (3)	121
O1W—H1W1···F1ii	0.85	1.97	2.550 (3)	125
O2W—H1W2···F3ii	0.85	2.10	2.664 (4)	124
O2W—H2W2···O3Wiii	0.85	2.33	2.730 (5)	110
O3W—H2W3···F2iv	0.80	1.98	2.767 (3)	171
O3W—H2W3···F3iv	0.80	2.96	3.490 (4)	126
O3W—H1W3···O3Wv	0.84	2.18	2.748	125

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O1W—H2W1⋯F1	0.85	2.22	2.699 (3)	116
O1W—H2W1⋯F2i	0.85	2.02	2.567 (3)	121
O1W—H2W1⋯F2i	0.85	2.02	2.567 (3)	121
O1W—H1W1⋯F1ii	0.85	1.97	2.550 (3)	125
O2W—H1W2⋯F3ii	0.85	2.10	2.664 (4)	124
O2W—H2W2⋯O3Wiii	0.85	2.33	2.730 (5)	110
O3W—H2W3⋯F2iv	0.80	1.98	2.767 (3)	171
O3W—H1W3⋯O3Wv	0.84	2.18	2.748 (7)	125

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .