cis-Dichloridobis(1,10-phenanthroline)chromium(III) chloride.

In the title complex, [CrCl(2)(C(12)H(8)N(2))(2)]Cl, the Cr(III) ion is situated on a twofold rotation axis and displays a slightly distorted octa-hedral CrCl(2)N(4) coordination geometry. The Cr environment is composed of a cis arrangement of two 1,10-phenanthroline and two chloride ligands. The chloride counter-anion exhibits half-occupation and is equally disordered over two positions.

Related literature

For background to chromium(III) complexes, see: Vincent (2000 ▶). For the structure of a related Cr(III) complex with phenanthroline ligands, see: Birk et al. (2008 ▶).

Experimental

Crystal data

[CrCl2(C12H8N2)2]Cl

M = 518.76

Monoclinic,

a = 15.446 (7) Å

b = 13.762 (6) Å

c = 12.536 (5) Å

β = 100.398 (6)°

V = 2621.1 (19) Å3

Z = 4

Mo Kα radiation

μ = 0.76 mm−1

T = 298 K

0.40 × 0.10 × 0.10 mm

Data collection

Bruker SMART CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 2000 ▶) T min = 0.751, T max = 0.928

5182 measured reflections

2265 independent reflections

1778 reflections with I > 2σ(I)

R int = 0.039

Refinement

R[F 2 > 2σ(F 2)] = 0.070

wR(F 2) = 0.211

S = 1.07

2265 reflections

150 parameters

H-atom parameters constrained

Δρmax = 0.92 e Å−3

Δρmin = −0.35 e Å−3

Data collection: SMART (Bruker, 2000 ▶); cell refinement: SAINT (Bruker, 2000 ▶); 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 I, global. DOI: 10.1107/S1600536810053845/wm2436sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810053845/wm2436Isup2.hkl

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

[CrCl2(C12H8N2)2]Cl	F(000) = 1052
Mr = 518.76	Dx = 1.315 Mg m−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 1354 reflections
a = 15.446 (7) Å	θ = 2.7–19.9°
b = 13.762 (6) Å	µ = 0.76 mm−1
c = 12.536 (5) Å	T = 298 K
β = 100.398 (6)°	Block, red
V = 2621.1 (19) Å3	0.40 × 0.10 × 0.10 mm
Z = 4

Bruker SMART CCD area-detector diffractometer	2265 independent reflections
Radiation source: fine-focus sealed tube	1778 reflections with I > 2σ(I)
graphite	Rint = 0.039
φ and ω scans	θmax = 25.0°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 2000)	h = −18→18
Tmin = 0.751, Tmax = 0.928	k = −16→16
5182 measured reflections	l = −7→14

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)] = 0.070	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.211	H-atom parameters constrained
S = 1.07	w = 1/[σ2(Fo2) + (0.1164P)2 + 5.5982P] where P = (Fo2 + 2Fc2)/3
2265 reflections	(Δ/σ)max < 0.001
150 parameters	Δρmax = 0.92 e Å−3
0 restraints	Δρmin = −0.35 e Å−3

Experimental. the Cl-counter anion is only half occupied and equally disordered over two positions.

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	Occ. (<1)
Cr1	0.5000	0.83468 (7)	0.7500	0.0338 (4)
Cl1	0.60948 (7)	0.94883 (9)	0.76093 (10)	0.0481 (4)
N1	0.5196 (2)	0.8199 (3)	0.9163 (3)	0.0386 (9)
N2	0.5952 (2)	0.7267 (3)	0.7714 (3)	0.0383 (9)
C1	0.6878 (3)	0.6322 (4)	0.9120 (4)	0.0467 (12)
C2	0.7141 (4)	0.6151 (4)	1.0254 (5)	0.0600 (14)
H2	0.7577	0.5695	1.0490	0.072*
C3	0.6771 (4)	0.6636 (4)	1.0997 (5)	0.0576 (14)
H3	0.6957	0.6507	1.1731	0.069*
C4	0.6099 (3)	0.7344 (4)	1.0672 (4)	0.0495 (12)
C5	0.5685 (4)	0.7889 (4)	1.1387 (4)	0.0582 (14)
H5	0.5837	0.7789	1.2131	0.070*
C6	0.5068 (4)	0.8555 (4)	1.0999 (4)	0.0555 (14)
H6	0.4806	0.8923	1.1475	0.067*
C7	0.4820 (3)	0.8693 (4)	0.9869 (4)	0.0478 (12)
H7	0.4381	0.9142	0.9612	0.057*
C8	0.5826 (3)	0.7539 (3)	0.9552 (4)	0.0380 (10)
C9	0.6226 (3)	0.7021 (3)	0.8779 (4)	0.0370 (10)
C10	0.7257 (4)	0.5865 (4)	0.8319 (5)	0.0588 (14)
H10	0.7682	0.5387	0.8506	0.071*
C11	0.6995 (4)	0.6130 (5)	0.7255 (5)	0.0650 (16)
H11	0.7250	0.5839	0.6718	0.078*
C12	0.6345 (4)	0.6836 (4)	0.6980 (5)	0.0531 (13)
H12	0.6180	0.7012	0.6255	0.064*
Cl2	0.6999 (6)	0.6655 (4)	0.4261 (5)	0.157 (3)	0.50

	U11	U22	U33	U12	U13	U23
Cr1	0.0324 (6)	0.0364 (6)	0.0334 (6)	0.000	0.0081 (4)	0.000
Cl1	0.0390 (7)	0.0488 (7)	0.0549 (8)	−0.0079 (5)	0.0043 (5)	0.0066 (5)
N1	0.040 (2)	0.041 (2)	0.037 (2)	−0.0041 (17)	0.0121 (17)	−0.0010 (16)
N2	0.0376 (19)	0.039 (2)	0.040 (2)	0.0022 (16)	0.0107 (16)	0.0015 (17)
C1	0.040 (3)	0.047 (3)	0.053 (3)	0.002 (2)	0.007 (2)	0.006 (2)
C2	0.053 (3)	0.062 (3)	0.061 (3)	0.012 (3)	−0.001 (3)	0.015 (3)
C3	0.057 (3)	0.064 (4)	0.046 (3)	0.000 (3)	−0.005 (3)	0.010 (3)
C4	0.051 (3)	0.055 (3)	0.041 (3)	−0.009 (2)	0.004 (2)	−0.001 (2)
C5	0.070 (4)	0.068 (4)	0.037 (3)	−0.005 (3)	0.009 (2)	0.001 (3)
C6	0.069 (3)	0.062 (3)	0.039 (3)	−0.002 (3)	0.020 (3)	−0.012 (2)
C7	0.054 (3)	0.047 (3)	0.045 (3)	0.004 (2)	0.016 (2)	−0.005 (2)
C8	0.035 (2)	0.041 (2)	0.038 (2)	−0.0057 (19)	0.0053 (18)	0.0008 (19)
C9	0.034 (2)	0.036 (2)	0.041 (2)	−0.0036 (18)	0.0070 (19)	0.001 (2)
C10	0.052 (3)	0.055 (3)	0.071 (4)	0.021 (3)	0.016 (3)	0.008 (3)
C11	0.070 (4)	0.064 (4)	0.068 (4)	0.025 (3)	0.031 (3)	−0.004 (3)
C12	0.059 (3)	0.057 (3)	0.047 (3)	0.011 (3)	0.020 (3)	−0.002 (2)
Cl2	0.265 (8)	0.125 (4)	0.101 (4)	−0.037 (5)	0.086 (5)	−0.027 (3)

Cr1—N1	2.062 (4)	C3—C4	1.428 (8)
Cr1—N1i	2.062 (4)	C3—H3	0.9300
Cr1—N2i	2.073 (4)	C4—C5	1.408 (8)
Cr1—N2	2.073 (4)	C4—C8	1.417 (7)
Cr1—Cl1	2.2941 (15)	C5—C6	1.348 (8)
Cr1—Cl1i	2.2941 (15)	C5—H5	0.9300
N1—C7	1.330 (6)	C6—C7	1.411 (7)
N1—C8	1.356 (6)	C6—H6	0.9300
N2—C12	1.330 (6)	C7—H7	0.9300
N2—C9	1.368 (6)	C8—C9	1.431 (6)
C1—C10	1.399 (8)	C10—C11	1.372 (8)
C1—C9	1.403 (7)	C10—H10	0.9300
C1—C2	1.426 (8)	C11—C12	1.395 (8)
C2—C3	1.353 (8)	C11—H11	0.9300
C2—H2	0.9300	C12—H12	0.9300
N1—Cr1—N1i	168.7 (2)	C4—C3—H3	119.5
N1—Cr1—N2i	91.81 (14)	C5—C4—C8	116.2 (5)
N1i—Cr1—N2i	80.07 (15)	C5—C4—C3	124.9 (5)
N1—Cr1—N2	80.07 (15)	C8—C4—C3	118.9 (5)
N1i—Cr1—N2	91.81 (14)	C6—C5—C4	120.4 (5)
N2i—Cr1—N2	88.5 (2)	C6—C5—H5	119.8
N1—Cr1—Cl1	92.00 (11)	C4—C5—H5	119.8
N1i—Cr1—Cl1	95.73 (11)	C5—C6—C7	120.0 (5)
N2i—Cr1—Cl1	175.09 (11)	C5—C6—H6	120.0
N2—Cr1—Cl1	89.14 (11)	C7—C6—H6	120.0
N1—Cr1—Cl1i	95.73 (11)	N1—C7—C6	121.8 (5)
N1i—Cr1—Cl1i	92.00 (11)	N1—C7—H7	119.1
N2i—Cr1—Cl1i	89.14 (11)	C6—C7—H7	119.1
N2—Cr1—Cl1i	175.09 (10)	N1—C8—C4	123.3 (4)
Cl1—Cr1—Cl1i	93.56 (8)	N1—C8—C9	117.4 (4)
C7—N1—C8	118.3 (4)	C4—C8—C9	119.3 (4)
C7—N1—Cr1	128.4 (3)	N2—C9—C1	123.1 (4)
C8—N1—Cr1	113.2 (3)	N2—C9—C8	116.2 (4)
C12—N2—C9	117.7 (4)	C1—C9—C8	120.6 (4)
C12—N2—Cr1	129.2 (3)	C11—C10—C1	119.4 (5)
C9—N2—Cr1	113.0 (3)	C11—C10—H10	120.3
C10—C1—C9	117.3 (5)	C1—C10—H10	120.3
C10—C1—C2	124.2 (5)	C10—C11—C12	119.9 (5)
C9—C1—C2	118.5 (5)	C10—C11—H11	120.1
C3—C2—C1	121.7 (5)	C12—C11—H11	120.1
C3—C2—H2	119.1	N2—C12—C11	122.5 (5)
C1—C2—H2	119.1	N2—C12—H12	118.7
C2—C3—C4	121.1 (5)	C11—C12—H12	118.7
C2—C3—H3	119.5
N1i—Cr1—N1—C7	−137.2 (4)	Cr1—N1—C7—C6	−175.5 (4)
N2i—Cr1—N1—C7	−93.5 (4)	C5—C6—C7—N1	−1.8 (8)
N2—Cr1—N1—C7	178.4 (4)	C7—N1—C8—C4	0.4 (7)
Cl1—Cr1—N1—C7	89.6 (4)	Cr1—N1—C8—C4	177.3 (4)
Cl1i—Cr1—N1—C7	−4.2 (4)	C7—N1—C8—C9	−179.5 (4)
N1i—Cr1—N1—C8	46.3 (3)	Cr1—N1—C8—C9	−2.6 (5)
N2i—Cr1—N1—C8	90.0 (3)	C5—C4—C8—N1	−0.8 (7)
N2—Cr1—N1—C8	1.9 (3)	C3—C4—C8—N1	−179.7 (4)
Cl1—Cr1—N1—C8	−86.9 (3)	C5—C4—C8—C9	179.2 (4)
Cl1i—Cr1—N1—C8	179.3 (3)	C3—C4—C8—C9	0.2 (7)
N1—Cr1—N2—C12	−177.2 (5)	C12—N2—C9—C1	−1.9 (7)
N1i—Cr1—N2—C12	10.7 (4)	Cr1—N2—C9—C1	−178.7 (4)
N2i—Cr1—N2—C12	90.7 (4)	C12—N2—C9—C8	176.5 (4)
Cl1—Cr1—N2—C12	−85.0 (4)	Cr1—N2—C9—C8	−0.3 (5)
Cl1i—Cr1—N2—C12	151.5 (11)	C10—C1—C9—N2	0.1 (7)
N1—Cr1—N2—C9	−0.8 (3)	C2—C1—C9—N2	177.4 (5)
N1i—Cr1—N2—C9	−172.9 (3)	C10—C1—C9—C8	−178.3 (5)
N2i—Cr1—N2—C9	−92.9 (3)	C2—C1—C9—C8	−1.0 (7)
Cl1—Cr1—N2—C9	91.4 (3)	N1—C8—C9—N2	2.0 (6)
Cl1i—Cr1—N2—C9	−32.1 (15)	C4—C8—C9—N2	−178.0 (4)
C10—C1—C2—C3	177.9 (5)	N1—C8—C9—C1	−179.6 (4)
C9—C1—C2—C3	0.8 (8)	C4—C8—C9—C1	0.5 (7)
C1—C2—C3—C4	−0.1 (9)	C9—C1—C10—C11	1.4 (8)
C2—C3—C4—C5	−179.3 (6)	C2—C1—C10—C11	−175.7 (6)
C2—C3—C4—C8	−0.4 (8)	C1—C10—C11—C12	−1.2 (9)
C8—C4—C5—C6	−0.2 (8)	C9—N2—C12—C11	2.2 (8)
C3—C4—C5—C6	178.7 (5)	Cr1—N2—C12—C11	178.4 (4)
C4—C5—C6—C7	1.4 (9)	C10—C11—C12—N2	−0.7 (9)
C8—N1—C7—C6	0.9 (7)

Table 1

Selected bond lengths (Å)

Cr1—N1	2.062 (4)
Cr1—N2	2.073 (4)
Cr1—Cl1	2.2941 (15)