Trichloro­(1,4,7-trimethyl-1,4,7-triaza­cyclo­nonane)­chromium(III)

The structure of the title complex, [CrCl₃(C₉H₂₁N₃)], contains a distorted octa­hedral chromium(III) centre. The facial tridentate N-coordinating 1,4,7-trimethyl-1,4,7-triaza­cyclo­nonane ligand and three chloride ions make up the first coordination sphere.

Key indicators

• Single-crystal X-ray study
• T = 122 K
• Mean [sigma](C-C)= 0.001 Å
• R factor = 0.027
• wR factor = 0.060
• Data-to-parameter ratio = 78.1

checkCIF/PLATON results

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Computing details

Data collection: COLLECT (Nonius, 1999); cell refinement: DIRAX (Duisenberg, 1992); data reduction: EVALCCD (Duisenberg, 1998); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: program (reference)?.

Trichloro(1,4,7-trimethyl-1,4,7-triazacyclononane)chromium(III)

Crystal data

[CrCl3(C9H21N3)]	F(000) = 684
Mr = 329.64	Dx = 1.594 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 43956 reflections
a = 12.1518 (14) Å	θ = 1.7–45.0°
b = 7.2055 (5) Å	µ = 1.39 mm^−1
c = 15.6894 (14) Å	T = 122 K
β = 90.212 (8)°	Prism, green
V = 1373.8 (2) Å^3	0.29 × 0.28 × 0.1 mm
Z = 4

Data collection

Nonius KappaCCD area-detector diffractometer	11318 independent reflections
Radiation source: fine-focus sealed tube	9167 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.043
ω and φ scans	θmax = 45.0°, θmin = 1.7°
Absorption correction: integration Gaussian integration (Coppens, 1970)	h = −24→23
Tmin = 0.760, Tmax = 0.917	k = −14→14
88493 measured reflections	l = −31→30

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)] = 0.027	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.060	H-atom parameters constrained
S = 1.12	w = 1/[σ^2(Fo^2) + (0.0185P)^2 + 0.4402P] where P = (Fo^2 + 2Fc^2)/3
11318 reflections	(Δ/σ)max = 0.001
145 parameters	Δρmax = 0.44 e Å^−3
0 restraints	Δρmin = −0.77 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
Cr	0.256054 (7)	0.452712 (13)	0.375662 (6)	0.00830 (2)
Cl1	0.132596 (13)	0.68198 (2)	0.417195 (13)	0.01747 (3)
Cl2	0.248702 (15)	0.53888 (3)	0.232551 (11)	0.01814 (3)
Cl3	0.408174 (12)	0.63832 (2)	0.402906 (11)	0.01338 (3)
N1	0.35766 (4)	0.21756 (7)	0.35197 (3)	0.00986 (7)
N2	0.25580 (4)	0.33879 (8)	0.50200 (3)	0.01208 (8)
N3	0.12641 (4)	0.25615 (8)	0.35801 (4)	0.01124 (8)
C1	0.44468 (5)	0.24679 (10)	0.28664 (4)	0.01490 (10)
H1A	0.4873	0.1323	0.2798	0.018*
H1B	0.4937	0.3472	0.3051	0.018*
H1C	0.4103	0.2801	0.2321	0.018*
C2	0.41405 (5)	0.17887 (9)	0.43469 (4)	0.01266 (9)
H2A	0.4693	0.2767	0.4462	0.015*
H2B	0.4529	0.0584	0.4313	0.015*
C3	0.33124 (6)	0.17325 (10)	0.50658 (4)	0.01506 (10)
H3A	0.2873	0.0578	0.5026	0.018*
H3B	0.3705	0.1729	0.5620	0.018*
C4	0.28755 (6)	0.47329 (12)	0.56991 (5)	0.01905 (12)
H4A	0.2854	0.4115	0.6255	0.023*
H4B	0.2360	0.5778	0.5697	0.023*
H4C	0.3622	0.5190	0.5592	0.023*
C5	0.13960 (5)	0.28082 (10)	0.51649 (4)	0.01469 (10)
H5A	0.0928	0.3921	0.5235	0.018*
H5B	0.1351	0.2065	0.5694	0.018*
C6	0.09795 (5)	0.16670 (9)	0.44177 (4)	0.01404 (10)
H6A	0.1309	0.0412	0.4442	0.017*
H6B	0.0171	0.1531	0.4459	0.017*
C7	0.02426 (6)	0.33204 (11)	0.31831 (5)	0.01803 (12)
H7A	−0.0304	0.2328	0.3127	0.022*
H7B	0.0414	0.3821	0.2618	0.022*
H7C	−0.0053	0.4311	0.3543	0.022*
C8	0.17376 (5)	0.11713 (10)	0.29768 (4)	0.01375 (10)
H8A	0.1789	0.1727	0.2401	0.017*
H8B	0.1243	0.0082	0.2941	0.017*
C9	0.28695 (5)	0.05496 (9)	0.32661 (4)	0.01293 (9)
H9A	0.2795	−0.0303	0.3757	0.016*
H9B	0.3231	−0.0138	0.2798	0.016*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cr	0.00723 (3)	0.00727 (3)	0.01041 (3)	0.00028 (3)	0.00065 (2)	0.00035 (3)
Cl1	0.01205 (6)	0.00896 (5)	0.03145 (9)	0.00154 (4)	0.00568 (5)	−0.00168 (5)
Cl2	0.01770 (6)	0.02210 (7)	0.01462 (6)	0.00059 (6)	−0.00155 (5)	0.00739 (5)
Cl3	0.01028 (5)	0.01176 (5)	0.01811 (6)	−0.00248 (4)	0.00040 (4)	−0.00061 (5)
N1	0.00902 (16)	0.01007 (18)	0.01049 (18)	0.00104 (14)	0.00022 (13)	−0.00062 (14)
N2	0.01156 (18)	0.0143 (2)	0.01040 (18)	−0.00063 (16)	0.00172 (14)	−0.00056 (16)
N3	0.00872 (17)	0.01021 (19)	0.0148 (2)	0.00023 (14)	−0.00057 (14)	−0.00073 (16)
C1	0.0127 (2)	0.0172 (3)	0.0148 (2)	0.00151 (19)	0.00495 (18)	−0.0013 (2)
C2	0.0104 (2)	0.0142 (2)	0.0134 (2)	0.00243 (17)	−0.00161 (17)	0.00147 (18)
C3	0.0153 (2)	0.0173 (3)	0.0126 (2)	0.0022 (2)	−0.00018 (18)	0.0046 (2)
C4	0.0196 (3)	0.0250 (3)	0.0125 (2)	−0.0043 (2)	0.0018 (2)	−0.0056 (2)
C5	0.0133 (2)	0.0165 (3)	0.0143 (2)	−0.00219 (19)	0.00530 (18)	0.0001 (2)
C6	0.0123 (2)	0.0117 (2)	0.0181 (3)	−0.00265 (18)	0.00345 (18)	0.00040 (19)
C7	0.0102 (2)	0.0170 (3)	0.0268 (3)	0.0015 (2)	−0.0051 (2)	0.0000 (2)
C8	0.0122 (2)	0.0136 (2)	0.0154 (2)	0.00004 (18)	−0.00197 (18)	−0.00426 (19)
C9	0.0125 (2)	0.0098 (2)	0.0166 (2)	0.00092 (17)	−0.00030 (17)	−0.00323 (18)

Geometric parameters (Å, º)

Cr—N1	2.1301 (5)	C2—H2B	0.9900
Cr—N2	2.1453 (6)	C3—H3A	0.9900
Cr—N3	2.1358 (6)	C3—H3B	0.9900
Cr—Cl1	2.3264 (2)	C4—H4A	0.9800
Cr—Cl2	2.3309 (3)	C4—H4B	0.9800
Cr—Cl3	2.3201 (3)	C4—H4C	0.9800
N1—C1	1.4904 (8)	C5—C6	1.5173 (10)
N1—C2	1.4916 (8)	C5—H5A	0.9900
N1—C9	1.5056 (8)	C5—H5B	0.9900
N2—C3	1.5060 (9)	C6—H6A	0.9900
N2—C4	1.4902 (9)	C6—H6B	0.9900
N2—C5	1.4908 (9)	C7—H7A	0.9800
N3—C6	1.5051 (9)	C7—H7B	0.9800
N3—C7	1.4907 (9)	C7—H7C	0.9800
N3—C8	1.4947 (8)	C8—C9	1.5147 (9)
C1—H1A	0.9800	C8—H8A	0.9900
C1—H1B	0.9800	C8—H8B	0.9900
C1—H1C	0.9800	C9—H9A	0.9900
C2—C3	1.5149 (9)	C9—H9B	0.9900
C2—H2A	0.9900
N1—Cr—N2	81.93 (2)	H2A—C2—H2B	108.1
N1—Cr—N3	82.97 (2)	N2—C3—C2	110.44 (5)
N3—Cr—N2	82.09 (2)	N2—C3—H3A	109.6
N1—Cr—Cl1	171.351 (16)	C2—C3—H3A	109.6
N2—Cr—Cl1	90.564 (17)	N2—C3—H3B	109.6
N3—Cr—Cl1	91.785 (17)	C2—C3—H3B	109.6
N1—Cr—Cl2	93.670 (16)	H3A—C3—H3B	108.1
N2—Cr—Cl2	172.604 (17)	N2—C4—H4A	109.5
N3—Cr—Cl2	91.497 (17)	N2—C4—H4B	109.5
N1—Cr—Cl3	91.649 (17)	H4A—C4—H4B	109.5
N2—Cr—Cl3	93.110 (17)	N2—C4—H4C	109.5
N3—Cr—Cl3	173.224 (16)	H4A—C4—H4C	109.5
Cl1—Cr—Cl2	93.335 (9)	H4B—C4—H4C	109.5
Cl3—Cr—Cl1	93.051 (10)	N2—C5—C6	110.33 (5)
Cl3—Cr—Cl2	92.956 (9)	N2—C5—H5A	109.6
C1—N1—C2	107.45 (5)	C6—C5—H5A	109.6
C1—N1—C9	109.51 (5)	N2—C5—H5B	109.6
C2—N1—C9	110.14 (5)	C6—C5—H5B	109.6
C1—N1—Cr	114.89 (4)	H5A—C5—H5B	108.1
C2—N1—Cr	105.16 (4)	N3—C6—C5	111.43 (5)
C9—N1—Cr	109.55 (4)	N3—C6—H6A	109.3
C4—N2—C5	108.43 (5)	C5—C6—H6A	109.3
C4—N2—C3	108.97 (6)	N3—C6—H6B	109.3
C5—N2—C3	110.34 (5)	C5—C6—H6B	109.3
C4—N2—Cr	114.24 (5)	H6A—C6—H6B	108.0
C5—N2—Cr	104.64 (4)	N3—C7—H7A	109.5
C3—N2—Cr	110.14 (4)	N3—C7—H7B	109.5
C7—N3—C8	107.65 (5)	H7A—C7—H7B	109.5
C7—N3—C6	109.16 (5)	N3—C7—H7C	109.5
C8—N3—C6	110.86 (5)	H7A—C7—H7C	109.5
C7—N3—Cr	115.06 (4)	H7B—C7—H7C	109.5
C8—N3—Cr	103.95 (4)	N3—C8—C9	111.09 (5)
C6—N3—Cr	110.03 (4)	N3—C8—H8A	109.4
N1—C1—H1A	109.5	C9—C8—H8A	109.4
N1—C1—H1B	109.5	N3—C8—H8B	109.4
H1A—C1—H1B	109.5	C9—C8—H8B	109.4
N1—C1—H1C	109.5	H8A—C8—H8B	108.0
H1A—C1—H1C	109.5	N1—C9—C8	111.45 (5)
H1B—C1—H1C	109.5	N1—C9—H9A	109.3
N1—C2—C3	110.40 (5)	C8—C9—H9A	109.3
N1—C2—H2A	109.6	N1—C9—H9B	109.3
C3—C2—H2A	109.6	C8—C9—H9B	109.3
N1—C2—H2B	109.6	H9A—C9—H9B	108.0
C3—C2—H2B	109.6