mer-Trichloro­(2,2',2''-terpyridine)chromium(III) dimethyl sulfoxide solvate

The title compound, mer-[CrCl₃(C₁₅H₁₁N₃)]·(CH₃)₂SO, adopts a distorted octa­hedral configuration about the Cr^III atom.

Key indicators

• Single-crystal X-ray study
• T = 101 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.029
• wR factor = 0.072
• Data-to-parameter ratio = 21.1

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) .        500 Ang.
PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000)         500 Deg.

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

   2 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
   0 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus and XPREP (Bruker, 2004); program(s) used to solve structure: SHELXL97 (Sheldrick, 1997); program(s) used to refine structure: SIR97 (Altomare et al., 1999); molecular graphics: DIAMOND (Brandenburg & Putz, 2004 or 2005); software used to prepare material for publication: WinGX (Farrugia, 1999).

mer-Trichloro(2,2',2''-terpyridine)chromium(III) dimethyl sulfoxide solvate

Crystal data

[CrCl3(C15H11N3)]·C2H6OS	Z = 2
Mr = 469.75	F(000) = 478
Triclinic, P1	Dx = 1.568 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71069 Å
a = 8.818 (5) Å	Cell parameters from 5417 reflections
b = 10.672 (5) Å	θ = 2.3–25.7°
c = 10.749 (5) Å	µ = 1.09 mm^−1
α = 95.501 (5)°	T = 101 K
β = 91.029 (5)°	Plate, green
γ = 98.580 (5)°	0.22 × 0.21 × 0.04 mm
V = 995.1 (9) Å^3

Data collection

Bruker X8 APEXII 4K Kappa CCD diffractometer	4262 reflections with I > 2σ(I)
Detector resolution: 512 pixels mm^-1	Rint = 0.027
ω and φ scans	θmax = 28.4°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Bruker, 2004)	h = −11→11
Tmin = 0.799, Tmax = 0.962	k = −14→13
13304 measured reflections	l = −14→14
4966 independent reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	H-atom parameters constrained
R[F^2 > 2σ(F^2)] = 0.029	w = 1/[σ^2(Fo^2) + (0.0289P)^2 + 0.5329P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.072	(Δ/σ)max = 0.001
S = 1.04	Δρmax = 0.40 e Å^−3
4966 reflections	Δρmin = −0.42 e Å^−3
235 parameters

Special details

Experimental. The intensity data was collected on a Bruker X8 Apex II 4 K Kappa CCD diffractometer using an exposure time of 20 s/frame. A total of 1264 frames were collected with a frame width of 0.5° covering up to θ = 28.36° with 99.4% completeness accomplished.

IR ν(C—N): 1316 cm^-1, ν(C ≐C): 1600 cm^-1 UV–Vis (DMSO) λ_max (nm) [ε (M^-1cm^-1)]: 602?(160), 447?(178), 417 ?(239).

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.

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

	x	y	z	Uiso*/Ueq
Cr1	0.31658 (3)	0.22951 (2)	0.79530 (2)	0.01091 (7)
Cl1	0.22090 (4)	0.20840 (4)	0.99415 (4)	0.01575 (9)
Cl2	0.29478 (5)	0.44177 (4)	0.81421 (4)	0.01910 (10)
Cl3	0.42210 (5)	0.23308 (4)	0.59853 (4)	0.01627 (9)
N1	0.10464 (15)	0.14964 (13)	0.71324 (12)	0.0118 (3)
N2	0.33217 (15)	0.04445 (13)	0.78285 (12)	0.0108 (3)
N3	0.53542 (15)	0.23265 (14)	0.87002 (13)	0.0134 (3)
C1	0.3380 (2)	0.40281 (19)	0.30294 (18)	0.0233 (4)
H1	0.3123	0.3611	0.2184	0.035*
H2	0.3638	0.34	0.3574	0.035*
H3	0.426	0.4703	0.3002	0.035*
C2	0.2620 (2)	0.53508 (18)	0.51085 (17)	0.0204 (4)
H4	0.188	0.5778	0.5592	0.031*
H5	0.3534	0.5967	0.4988	0.031*
H6	0.2913	0.4664	0.5561	0.031*
C11	−0.00496 (19)	0.21352 (17)	0.67530 (15)	0.0148 (3)
H11	0.0134	0.304	0.6842	0.018*
C12	−0.14512 (19)	0.15090 (18)	0.62315 (15)	0.0168 (3)
H12	−0.2212	0.1979	0.5968	0.02*
C13	−0.17133 (19)	0.01889 (17)	0.61041 (15)	0.0165 (3)
H13	−0.2665	−0.0255	0.576	0.02*
C14	−0.05834 (18)	−0.04815 (17)	0.64797 (15)	0.0142 (3)
H14	−0.0747	−0.1386	0.6394	0.017*
C15	0.07948 (18)	0.01980 (16)	0.69845 (14)	0.0118 (3)
C21	0.21143 (18)	−0.04047 (16)	0.73625 (14)	0.0120 (3)
C22	0.21982 (19)	−0.16959 (16)	0.72502 (15)	0.0152 (3)
H22	0.1347	−0.23	0.6927	0.018*
C23	0.3564 (2)	−0.20895 (17)	0.76234 (16)	0.0167 (3)
H23	0.3649	−0.297	0.7551	0.02*
C24	0.47994 (19)	−0.11972 (17)	0.80999 (15)	0.0155 (3)
H24	0.5733	−0.1458	0.8352	0.019*
C25	0.46398 (18)	0.00823 (16)	0.82001 (14)	0.0119 (3)
C31	0.58044 (18)	0.11633 (16)	0.87010 (15)	0.0131 (3)
C32	0.72498 (19)	0.10266 (18)	0.91510 (15)	0.0165 (3)
H31	0.7542	0.0206	0.916	0.02*
C33	0.82601 (19)	0.21105 (19)	0.95880 (16)	0.0197 (4)
H32	0.9261	0.2041	0.9889	0.024*
C34	0.7798 (2)	0.32905 (19)	0.95810 (16)	0.0204 (4)
H33	0.8479	0.4041	0.9873	0.024*
C35	0.63283 (19)	0.33666 (18)	0.91420 (16)	0.0177 (4)
H34	0.6004	0.4178	0.9155	0.021*
O1	0.05939 (15)	0.35917 (13)	0.38844 (14)	0.0288 (3)
S1	0.17738 (5)	0.47014 (4)	0.36251 (4)	0.01838 (10)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.01000 (13)	0.01000 (14)	0.01206 (13)	0.00050 (10)	−0.00211 (9)	−0.00023 (10)
Cl1	0.01276 (18)	0.0224 (2)	0.01247 (18)	0.00490 (15)	−0.00096 (14)	0.00041 (15)
Cl2	0.0235 (2)	0.0113 (2)	0.0220 (2)	0.00283 (16)	−0.00179 (16)	−0.00078 (15)
Cl3	0.01678 (19)	0.0171 (2)	0.01427 (19)	−0.00018 (15)	0.00109 (14)	0.00230 (15)
N1	0.0116 (6)	0.0121 (7)	0.0114 (6)	0.0012 (5)	−0.0007 (5)	0.0008 (5)
N2	0.0099 (6)	0.0124 (7)	0.0096 (6)	0.0011 (5)	−0.0003 (5)	0.0002 (5)
N3	0.0109 (6)	0.0157 (7)	0.0127 (7)	0.0005 (5)	−0.0007 (5)	−0.0002 (5)
C1	0.0222 (9)	0.0253 (10)	0.0223 (9)	0.0060 (8)	0.0028 (7)	−0.0024 (8)
C2	0.0185 (9)	0.0187 (9)	0.0215 (9)	−0.0014 (7)	0.0009 (7)	−0.0036 (7)
C11	0.0157 (8)	0.0157 (8)	0.0129 (8)	0.0032 (7)	−0.0009 (6)	0.0012 (6)
C12	0.0140 (8)	0.0233 (9)	0.0140 (8)	0.0060 (7)	−0.0022 (6)	0.0021 (7)
C13	0.0122 (8)	0.0220 (9)	0.0138 (8)	−0.0001 (7)	−0.0012 (6)	−0.0016 (7)
C14	0.0135 (8)	0.0148 (8)	0.0127 (8)	−0.0009 (6)	0.0002 (6)	−0.0018 (6)
C15	0.0121 (7)	0.0129 (8)	0.0098 (7)	0.0012 (6)	0.0002 (6)	−0.0007 (6)
C21	0.0105 (7)	0.0144 (8)	0.0106 (7)	0.0004 (6)	0.0006 (6)	0.0008 (6)
C22	0.0159 (8)	0.0129 (8)	0.0157 (8)	0.0002 (6)	−0.0008 (6)	−0.0004 (6)
C23	0.0214 (9)	0.0121 (8)	0.0168 (8)	0.0043 (7)	−0.0003 (6)	0.0001 (6)
C24	0.0147 (8)	0.0187 (9)	0.0143 (8)	0.0069 (7)	−0.0009 (6)	0.0010 (6)
C25	0.0113 (7)	0.0154 (8)	0.0088 (7)	0.0025 (6)	0.0007 (5)	0.0000 (6)
C31	0.0106 (7)	0.0179 (9)	0.0105 (7)	0.0016 (6)	0.0006 (6)	0.0003 (6)
C32	0.0130 (8)	0.0227 (9)	0.0139 (8)	0.0039 (7)	0.0016 (6)	0.0002 (7)
C33	0.0094 (8)	0.0330 (11)	0.0157 (8)	0.0019 (7)	−0.0008 (6)	−0.0008 (7)
C34	0.0133 (8)	0.0256 (10)	0.0185 (9)	−0.0056 (7)	−0.0010 (6)	−0.0035 (7)
C35	0.0161 (8)	0.0171 (9)	0.0178 (8)	−0.0021 (7)	−0.0006 (6)	−0.0011 (7)
O1	0.0149 (6)	0.0177 (7)	0.0498 (9)	−0.0038 (5)	−0.0011 (6)	−0.0064 (6)
S1	0.0151 (2)	0.0149 (2)	0.0243 (2)	0.00200 (16)	−0.00522 (16)	−0.00089 (17)

Geometric parameters (Å, º)

Cr1—N2	1.9921 (17)	C12—H12	0.95
Cr1—N3	2.0712 (17)	C13—C14	1.386 (3)
Cr1—N1	2.0782 (16)	C13—H13	0.95
Cr1—Cl2	2.2919 (12)	C14—C15	1.391 (2)
Cr1—Cl3	2.3272 (10)	C14—H14	0.95
Cr1—Cl1	2.3306 (11)	C15—C21	1.479 (2)
N1—C11	1.342 (2)	C21—C22	1.385 (2)
N1—C15	1.363 (2)	C22—C23	1.398 (2)
N2—C25	1.344 (2)	C22—H22	0.95
N2—C21	1.346 (2)	C23—C24	1.390 (2)
N3—C35	1.340 (2)	C23—H23	0.95
N3—C31	1.359 (2)	C24—C25	1.388 (3)
C1—S1	1.783 (2)	C24—H24	0.95
C1—H1	0.98	C25—C31	1.477 (2)
C1—H2	0.98	C31—C32	1.388 (2)
C1—H3	0.98	C32—C33	1.388 (3)
C2—S1	1.7808 (19)	C32—H31	0.95
C2—H4	0.98	C33—C34	1.381 (3)
C2—H5	0.98	C33—H32	0.95
C2—H6	0.98	C34—C35	1.388 (3)
C11—C12	1.395 (2)	C34—H33	0.95
C11—H11	0.95	C35—H34	0.95
C12—C13	1.386 (3)	O1—S1	1.5063 (15)
N2—Cr1—N3	78.61 (6)	C14—C13—C12	119.85 (16)
N2—Cr1—N1	78.42 (6)	C14—C13—H13	120.1
N3—Cr1—N1	157.02 (6)	C12—C13—H13	120.1
N2—Cr1—Cl2	178.48 (4)	C13—C14—C15	118.62 (16)
N3—Cr1—Cl2	101.70 (4)	C13—C14—H14	120.7
N1—Cr1—Cl2	101.28 (5)	C15—C14—H14	120.7
N2—Cr1—Cl3	87.32 (4)	N1—C15—C14	121.70 (15)
N3—Cr1—Cl3	88.26 (5)	N1—C15—C21	114.51 (14)
N1—Cr1—Cl3	90.03 (5)	C14—C15—C21	123.76 (16)
Cl2—Cr1—Cl3	94.174 (19)	N2—C21—C22	120.40 (15)
N2—Cr1—Cl1	87.61 (4)	N2—C21—C15	113.11 (15)
N3—Cr1—Cl1	88.83 (5)	C22—C21—C15	126.47 (14)
N1—Cr1—Cl1	90.86 (5)	C21—C22—C23	118.44 (15)
Cl2—Cr1—Cl1	90.90 (2)	C21—C22—H22	120.8
Cl3—Cr1—Cl1	174.57 (2)	C23—C22—H22	120.8
C11—N1—C15	119.13 (14)	C24—C23—C22	120.27 (17)
C11—N1—Cr1	126.20 (12)	C24—C23—H23	119.9
C15—N1—Cr1	114.66 (11)	C22—C23—H23	119.9
C25—N2—C21	121.95 (15)	C25—C24—C23	118.58 (16)
C25—N2—Cr1	118.86 (11)	C25—C24—H24	120.7
C21—N2—Cr1	119.19 (11)	C23—C24—H24	120.7
C35—N3—C31	119.28 (15)	N2—C25—C24	120.36 (15)
C35—N3—Cr1	126.13 (13)	N2—C25—C31	113.10 (15)
C31—N3—Cr1	114.58 (11)	C24—C25—C31	126.55 (15)
S1—C1—H1	109.5	N3—C31—C32	121.53 (15)
S1—C1—H2	109.5	N3—C31—C25	114.80 (14)
H1—C1—H2	109.5	C32—C31—C25	123.66 (16)
S1—C1—H3	109.5	C33—C32—C31	118.79 (18)
H1—C1—H3	109.5	C33—C32—H31	120.6
H2—C1—H3	109.5	C31—C32—H31	120.6
S1—C2—H4	109.5	C34—C33—C32	119.41 (17)
S1—C2—H5	109.5	C34—C33—H32	120.3
H4—C2—H5	109.5	C32—C33—H32	120.3
S1—C2—H6	109.5	C33—C34—C35	119.23 (17)
H4—C2—H6	109.5	C33—C34—H33	120.4
H5—C2—H6	109.5	C35—C34—H33	120.4
N1—C11—C12	121.88 (16)	N3—C35—C34	121.74 (18)
N1—C11—H11	119.1	N3—C35—H34	119.1
C12—C11—H11	119.1	C34—C35—H34	119.1
C13—C12—C11	118.80 (16)	O1—S1—C2	105.68 (9)
C13—C12—H12	120.6	O1—S1—C1	105.87 (10)
C11—C12—H12	120.6	C2—S1—C1	97.38 (9)
N2—Cr1—N1—C11	−177.01 (14)	Cr1—N1—C15—C21	−3.64 (17)
N3—Cr1—N1—C11	−175.38 (13)	C13—C14—C15—N1	0.9 (2)
Cl2—Cr1—N1—C11	4.52 (13)	C13—C14—C15—C21	−176.93 (15)
Cl3—Cr1—N1—C11	−89.75 (13)	C25—N2—C21—C22	−0.1 (2)
Cl1—Cr1—N1—C11	95.61 (13)	Cr1—N2—C21—C22	179.16 (12)
N2—Cr1—N1—C15	3.03 (11)	C25—N2—C21—C15	−178.66 (13)
N3—Cr1—N1—C15	4.7 (2)	Cr1—N2—C21—C15	0.55 (17)
Cl2—Cr1—N1—C15	−175.44 (10)	N1—C15—C21—N2	2.10 (19)
Cl3—Cr1—N1—C15	90.29 (11)	C14—C15—C21—N2	−179.89 (14)
Cl1—Cr1—N1—C15	−84.35 (11)	N1—C15—C21—C22	−176.40 (15)
N3—Cr1—N2—C25	−2.04 (11)	C14—C15—C21—C22	1.6 (3)
N1—Cr1—N2—C25	177.32 (12)	N2—C21—C22—C23	−0.4 (2)
Cl3—Cr1—N2—C25	86.73 (11)	C15—C21—C22—C23	177.99 (15)
Cl1—Cr1—N2—C25	−91.32 (11)	C21—C22—C23—C24	0.3 (2)
N3—Cr1—N2—C21	178.73 (12)	C22—C23—C24—C25	0.3 (2)
N1—Cr1—N2—C21	−1.92 (11)	C21—N2—C25—C24	0.7 (2)
Cl3—Cr1—N2—C21	−92.50 (12)	Cr1—N2—C25—C24	−178.54 (12)
Cl1—Cr1—N2—C21	89.45 (12)	C21—N2—C25—C31	−178.99 (13)
N2—Cr1—N3—C35	−179.43 (14)	Cr1—N2—C25—C31	1.79 (17)
N1—Cr1—N3—C35	178.94 (13)	C23—C24—C25—N2	−0.8 (2)
Cl2—Cr1—N3—C35	−0.95 (14)	C23—C24—C25—C31	178.84 (15)
Cl3—Cr1—N3—C35	92.95 (13)	C35—N3—C31—C32	0.1 (2)
Cl1—Cr1—N3—C35	−91.63 (13)	Cr1—N3—C31—C32	178.89 (12)
N2—Cr1—N3—C31	1.89 (11)	C35—N3—C31—C25	179.69 (14)
N1—Cr1—N3—C31	0.3 (2)	Cr1—N3—C31—C25	−1.53 (17)
Cl2—Cr1—N3—C31	−179.63 (10)	N2—C25—C31—N3	−0.1 (2)
Cl3—Cr1—N3—C31	−85.73 (11)	C24—C25—C31—N3	−179.73 (15)
Cl1—Cr1—N3—C31	89.69 (11)	N2—C25—C31—C32	179.48 (14)
C15—N1—C11—C12	1.2 (2)	C24—C25—C31—C32	−0.2 (3)
Cr1—N1—C11—C12	−178.79 (12)	N3—C31—C32—C33	−1.1 (2)
N1—C11—C12—C13	0.0 (2)	C25—C31—C32—C33	179.32 (15)
C11—C12—C13—C14	−0.7 (2)	C31—C32—C33—C34	0.9 (2)
C12—C13—C14—C15	0.3 (2)	C32—C33—C34—C35	0.3 (3)
C11—N1—C15—C14	−1.7 (2)	C31—N3—C35—C34	1.2 (2)
Cr1—N1—C15—C14	178.31 (12)	Cr1—N3—C35—C34	−177.45 (12)
C11—N1—C15—C21	176.40 (13)	C33—C34—C35—N3	−1.4 (3)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1···Cl1^i	0.98	2.81	3.782 (2)	171
C2—H4···O1^ii	0.98	2.44	3.363 (3)	158
C2—H5···Cl3^iii	0.98	2.77	3.726 (2)	165
C14—H14···O1^iv	0.95	2.37	3.303 (3)	168
C22—H22···O1^iv	0.95	2.15	3.094 (2)	177
C24—H24···Cl1^v	0.95	2.75	3.635 (2)	155
C32—H31···Cl1^v	0.95	2.75	3.644 (2)	157
C33—H32···Cl1^vi	0.95	2.59	3.501 (3)	160

Symmetry codes: (i) x, y, z−1; (ii) −x, −y+1, −z+1; (iii) −x+1, −y+1, −z+1; (iv) −x, −y, −z+1; (v) −x+1, −y, −z+2; (vi) x+1, y, z.