[Bis(2-methyl-1-pyrid­yl)phenyl­phosphine-κ²N,P,N′]trichloro­chromium(III) acetonitrile solvate

In the title mol­ecular structure, [CrCl₃{PPh(2-CH₂C₅H₄N)₂}]·CH₃CN, the Cr^III atom exhibits an octa­hedral coordination geometry, with a tridentate ligand capping one face of the octa­hedron and three Cl⁻ ions occupying the opposite face.

Key indicators

• Single-crystal X-ray study
• T = 110 K
• Mean [sigma](C-C)= 0.003 Å
• R factor = 0.039
• wR factor = 0.086
• Data-to-parameter ratio = 21.6

checkCIF/PLATON results

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Computing details

Data collection: APEX2 (Bruker, 2003); cell refinement: SAINT-Plus (Bruker, 2003); 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 (Sheldrick, 2000); software used to prepare material for publication: SHELXTL.

[Bis(2-methyl-1-pyridyl)phenylphosphine-κ²N,P,N']trichlorochromium(III) acetonitrile solvate

Crystal data

[CrCl3(C18H17N2P)]·C2H3N	F(000) = 1004
Mr = 491.71	Dx = 1.476 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 5658 reflections
a = 11.0206 (12) Å	θ = 2.5–28.3°
b = 16.1145 (16) Å	µ = 0.96 mm^−1
c = 13.0390 (14) Å	T = 110 K
β = 107.081 (4)°	Block, green
V = 2213.5 (4) Å^3	0.27 × 0.19 × 0.16 mm
Z = 4

Data collection

Bruker APEX X8 diffractometer	5487 independent reflections
Radiation source: fine-focus sealed tube	4230 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.044
φ and ω scans	θmax = 28.3°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −14→13
Tmin = 0.697, Tmax = 0.859	k = −19→21
21619 measured reflections	l = −15→17

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)] = 0.039	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.086	H-atom parameters constrained
S = 1.03	w = 1/[σ^2(Fo^2) + (0.035P)^2 + 0.906P] where P = (Fo^2 + 2Fc^2)/3
5487 reflections	(Δ/σ)max = 0.001
254 parameters	Δρmax = 0.46 e Å^−3
0 restraints	Δρmin = −0.40 e Å^−3

Special details

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.

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

	x	y	z	Uiso*/Ueq
Cr1	0.41325 (3)	0.77207 (2)	0.44412 (3)	0.01493 (9)
Cl1	0.19752 (5)	0.74352 (4)	0.36894 (5)	0.02619 (14)
Cl2	0.40570 (5)	0.90443 (3)	0.37308 (5)	0.02282 (13)
Cl3	0.47528 (5)	0.70814 (3)	0.30821 (4)	0.02016 (13)
P1	0.62565 (5)	0.80224 (3)	0.53745 (5)	0.01519 (12)
N1	0.45945 (17)	0.66045 (11)	0.53554 (14)	0.0166 (4)
N2	0.38878 (17)	0.82477 (11)	0.58778 (15)	0.0185 (4)
N3	1.1039 (2)	0.43484 (15)	0.45648 (18)	0.0378 (6)
C1	0.6837 (2)	0.70492 (13)	0.60459 (18)	0.0197 (5)
H1A	0.7417	0.6796	0.5704	0.024*
H1B	0.7306	0.7162	0.6787	0.024*
C2	0.5780 (2)	0.64521 (13)	0.60150 (17)	0.0183 (5)
C3	0.3696 (2)	0.60152 (14)	0.52877 (18)	0.0224 (5)
H3	0.2883	0.6109	0.4833	0.027*
C4	0.3930 (2)	0.52845 (15)	0.5861 (2)	0.0278 (6)
H4	0.3289	0.4894	0.5788	0.033*
C5	0.5126 (3)	0.51414 (15)	0.6543 (2)	0.0279 (6)
H5	0.5303	0.4655	0.6944	0.033*
C6	0.6059 (2)	0.57316 (14)	0.66229 (19)	0.0245 (5)
H6	0.6872	0.5646	0.7082	0.029*
C7	0.6085 (2)	0.87703 (14)	0.63667 (18)	0.0202 (5)
H7A	0.6773	0.8700	0.7024	0.024*
H7B	0.6136	0.9328	0.6103	0.024*
C8	0.4837 (2)	0.86573 (13)	0.65954 (18)	0.0185 (5)
C9	0.2758 (2)	0.81771 (15)	0.60906 (19)	0.0236 (5)
H9	0.2101	0.7896	0.5602	0.028*
C10	0.2542 (2)	0.85037 (15)	0.6999 (2)	0.0281 (6)
H10	0.1755	0.8442	0.7118	0.034*
C11	0.3511 (2)	0.89243 (15)	0.77296 (19)	0.0273 (6)
H11	0.3388	0.9151	0.8348	0.033*
C12	0.4662 (2)	0.90012 (14)	0.75230 (18)	0.0235 (5)
H12	0.5324	0.9284	0.8004	0.028*
C13	0.7447 (2)	0.84172 (14)	0.48005 (18)	0.0184 (5)
C14	0.8097 (2)	0.78666 (16)	0.4328 (2)	0.0262 (5)
H14	0.7921	0.7302	0.4320	0.031*
C15	0.9002 (2)	0.81526 (17)	0.3870 (2)	0.0328 (6)
H15	0.9435	0.7780	0.3559	0.039*
C16	0.9262 (2)	0.89906 (18)	0.3873 (2)	0.0354 (6)
H16	0.9885	0.9182	0.3581	0.042*
C17	0.8596 (2)	0.95451 (17)	0.4312 (2)	0.0321 (6)
H17	0.8757	1.0111	0.4297	0.039*
C18	0.7685 (2)	0.92631 (15)	0.47742 (19)	0.0257 (5)
H18	0.7237	0.9639	0.5065	0.031*
C19	1.0144 (2)	0.40999 (15)	0.3965 (2)	0.0259 (5)
C20	0.9009 (3)	0.37760 (18)	0.3186 (2)	0.0371 (6)
H20A	0.9197	0.3249	0.2926	0.056*
H20B	0.8734	0.4157	0.2597	0.056*
H20C	0.8348	0.3709	0.3522	0.056*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr1	0.01502 (17)	0.01649 (18)	0.01413 (19)	0.00046 (13)	0.00560 (14)	−0.00183 (14)
Cl1	0.0160 (3)	0.0385 (3)	0.0235 (3)	−0.0024 (2)	0.0048 (2)	−0.0072 (3)
Cl2	0.0284 (3)	0.0178 (3)	0.0217 (3)	0.0049 (2)	0.0065 (2)	0.0016 (2)
Cl3	0.0265 (3)	0.0187 (3)	0.0187 (3)	0.0013 (2)	0.0119 (2)	−0.0020 (2)
P1	0.0162 (3)	0.0132 (3)	0.0165 (3)	−0.0005 (2)	0.0053 (2)	−0.0009 (2)
N1	0.0209 (9)	0.0168 (9)	0.0147 (9)	−0.0028 (7)	0.0091 (8)	−0.0034 (7)
N2	0.0215 (10)	0.0177 (9)	0.0178 (10)	0.0031 (7)	0.0080 (8)	−0.0006 (8)
N3	0.0376 (13)	0.0453 (14)	0.0287 (13)	0.0127 (11)	0.0071 (11)	0.0018 (11)
C1	0.0197 (11)	0.0184 (11)	0.0194 (12)	0.0006 (9)	0.0035 (9)	0.0014 (9)
C2	0.0245 (12)	0.0178 (11)	0.0145 (11)	−0.0007 (9)	0.0088 (9)	−0.0050 (9)
C3	0.0265 (12)	0.0240 (12)	0.0195 (12)	−0.0058 (10)	0.0113 (10)	−0.0048 (10)
C4	0.0374 (14)	0.0230 (13)	0.0299 (14)	−0.0115 (11)	0.0206 (12)	−0.0030 (10)
C5	0.0476 (16)	0.0165 (12)	0.0243 (13)	−0.0023 (11)	0.0180 (12)	0.0009 (10)
C6	0.0340 (13)	0.0169 (11)	0.0223 (13)	0.0011 (10)	0.0079 (11)	−0.0007 (9)
C7	0.0249 (12)	0.0157 (11)	0.0199 (12)	−0.0017 (9)	0.0062 (10)	−0.0040 (9)
C8	0.0252 (12)	0.0135 (10)	0.0170 (12)	0.0036 (9)	0.0065 (9)	0.0003 (9)
C9	0.0249 (12)	0.0270 (13)	0.0221 (13)	0.0011 (10)	0.0120 (10)	0.0007 (10)
C10	0.0338 (14)	0.0310 (14)	0.0264 (14)	0.0055 (11)	0.0196 (11)	0.0031 (11)
C11	0.0421 (15)	0.0259 (13)	0.0183 (12)	0.0127 (11)	0.0156 (11)	0.0019 (10)
C12	0.0338 (13)	0.0189 (12)	0.0171 (12)	0.0049 (10)	0.0062 (10)	−0.0030 (9)
C13	0.0145 (10)	0.0219 (12)	0.0182 (12)	−0.0004 (9)	0.0039 (9)	0.0023 (9)
C14	0.0250 (12)	0.0282 (13)	0.0283 (14)	−0.0005 (10)	0.0121 (11)	−0.0012 (10)
C15	0.0245 (13)	0.0423 (16)	0.0364 (16)	−0.0014 (11)	0.0164 (12)	−0.0051 (12)
C16	0.0237 (13)	0.0521 (18)	0.0336 (16)	−0.0093 (12)	0.0136 (12)	0.0058 (13)
C17	0.0287 (13)	0.0292 (14)	0.0374 (16)	−0.0091 (11)	0.0081 (12)	0.0076 (12)
C18	0.0223 (12)	0.0259 (13)	0.0284 (14)	−0.0009 (10)	0.0066 (10)	0.0029 (10)
C19	0.0343 (14)	0.0239 (13)	0.0226 (13)	0.0107 (11)	0.0132 (12)	0.0057 (10)
C20	0.0353 (15)	0.0366 (15)	0.0420 (17)	−0.0041 (12)	0.0156 (13)	−0.0097 (13)

Geometric parameters (Å, º)

Cr1—N1	2.1352 (18)	C7—H7A	0.9700
Cr1—N2	2.1447 (18)	C7—H7B	0.9700
Cr1—Cl2	2.3171 (7)	C8—C12	1.395 (3)
Cr1—Cl3	2.3197 (6)	C9—C10	1.379 (3)
Cr1—Cl1	2.3358 (7)	C9—H9	0.9300
Cr1—P1	2.3502 (7)	C10—C11	1.382 (4)
P1—C13	1.807 (2)	C10—H10	0.9300
P1—C1	1.818 (2)	C11—C12	1.378 (3)
P1—C7	1.818 (2)	C11—H11	0.9300
N1—C3	1.356 (3)	C12—H12	0.9300
N1—C2	1.359 (3)	C13—C18	1.390 (3)
N2—C8	1.353 (3)	C13—C14	1.392 (3)
N2—C9	1.357 (3)	C14—C15	1.383 (3)
N3—C19	1.137 (3)	C14—H14	0.9300
C1—C2	1.503 (3)	C15—C16	1.380 (4)
C1—H1A	0.9700	C15—H15	0.9300
C1—H1B	0.9700	C16—C17	1.383 (4)
C2—C6	1.388 (3)	C16—H16	0.9300
C3—C4	1.378 (3)	C17—C18	1.390 (3)
C3—H3	0.9300	C17—H17	0.9300
C4—C5	1.376 (4)	C18—H18	0.9300
C4—H4	0.9300	C19—C20	1.457 (4)
C5—C6	1.382 (3)	C20—H20A	0.9600
C5—H5	0.9300	C20—H20B	0.9600
C6—H6	0.9300	C20—H20C	0.9600
C7—C8	1.501 (3)
N1—Cr1—N2	85.21 (7)	C2—C6—H6	120.1
N1—Cr1—Cl2	166.73 (5)	C8—C7—P1	110.70 (15)
N2—Cr1—Cl2	89.18 (5)	C8—C7—H7A	109.5
N1—Cr1—Cl3	88.68 (5)	P1—C7—H7A	109.5
N2—Cr1—Cl3	169.74 (5)	C8—C7—H7B	109.5
Cl2—Cr1—Cl3	95.01 (2)	P1—C7—H7B	109.5
N1—Cr1—Cl1	96.59 (5)	H7A—C7—H7B	108.1
N2—Cr1—Cl1	94.07 (5)	N2—C8—C12	121.1 (2)
Cl2—Cr1—Cl1	95.79 (2)	N2—C8—C7	119.30 (19)
Cl3—Cr1—Cl1	94.81 (2)	C12—C8—C7	119.5 (2)
N1—Cr1—P1	81.22 (5)	N2—C9—C10	122.9 (2)
N2—Cr1—P1	80.06 (5)	N2—C9—H9	118.5
Cl2—Cr1—P1	85.98 (2)	C10—C9—H9	118.5
Cl3—Cr1—P1	90.87 (2)	C9—C10—C11	119.1 (2)
Cl1—Cr1—P1	173.86 (3)	C9—C10—H10	120.5
C13—P1—C1	107.90 (10)	C11—C10—H10	120.5
C13—P1—C7	107.53 (10)	C12—C11—C10	118.6 (2)
C1—P1—C7	108.94 (11)	C12—C11—H11	120.7
C13—P1—Cr1	126.34 (8)	C10—C11—H11	120.7
C1—P1—Cr1	103.12 (7)	C11—C12—C8	120.3 (2)
C7—P1—Cr1	102.11 (8)	C11—C12—H12	119.9
C3—N1—C2	117.55 (19)	C8—C12—H12	119.9
C3—N1—Cr1	120.25 (15)	C18—C13—C14	119.3 (2)
C2—N1—Cr1	122.20 (14)	C18—C13—P1	121.36 (17)
C8—N2—C9	117.97 (19)	C14—C13—P1	119.30 (17)
C8—N2—Cr1	121.80 (14)	C15—C14—C13	120.6 (2)
C9—N2—Cr1	120.23 (16)	C15—C14—H14	119.7
C2—C1—P1	112.26 (15)	C13—C14—H14	119.7
C2—C1—H1A	109.2	C16—C15—C14	120.0 (2)
P1—C1—H1A	109.2	C16—C15—H15	120.0
C2—C1—H1B	109.2	C14—C15—H15	120.0
P1—C1—H1B	109.2	C15—C16—C17	119.9 (2)
H1A—C1—H1B	107.9	C15—C16—H16	120.1
N1—C2—C6	121.6 (2)	C17—C16—H16	120.1
N1—C2—C1	119.67 (19)	C16—C17—C18	120.5 (2)
C6—C2—C1	118.7 (2)	C16—C17—H17	119.8
N1—C3—C4	123.1 (2)	C18—C17—H17	119.8
N1—C3—H3	118.4	C17—C18—C13	119.8 (2)
C4—C3—H3	118.4	C17—C18—H18	120.1
C5—C4—C3	119.0 (2)	C13—C18—H18	120.1
C5—C4—H4	120.5	N3—C19—C20	179.1 (3)
C3—C4—H4	120.5	C19—C20—H20A	109.5
C4—C5—C6	118.9 (2)	C19—C20—H20B	109.5
C4—C5—H5	120.5	H20A—C20—H20B	109.5
C6—C5—H5	120.5	C19—C20—H20C	109.5
C5—C6—C2	119.8 (2)	H20A—C20—H20C	109.5
C5—C6—H6	120.1	H20B—C20—H20C	109.5