trans-Dichloridobis(propane-1,3-diamine-κN,N')chromium(III) perchlorate.

In the title compound, [CrCl(2)(C(3)H(10)N(2))(2)]ClO(4), the Cr(III) atom is coordinated equatorially by four N atoms of two propane-1,3-diamine (tn) ligands and axially by two mutually trans Cl atoms, thus displaying a slightly distorted octa-hedral geometry with no crystallographically imposed symmetry. The two six-membered chair chelate rings in the complex cation are in an anti conformation with respect to each other. The Cr-N bond lengths range from 2.0831 (18) to 2.0917 (19) Å, and the Cr-Cl bond lengths are 2.3148 (6) and 2.3135 (6) Å. The perchlorate anions have slightly distorted tetra-hedral geometries. Weak inter-molecular hydrogen bonds involving the tn ligand NH groups as donors, and chloride ligands and anion O atoms as acceptors are observed.

Related literature

For the synthesis, see: Couldwell & House (1972 ▶); House (1970 ▶). For related structures, see: Choi et al. (2002 ▶, 2007 ▶, 2008 ▶, 2010 ▶); Vaughn & Rogers (1985 ▶); Kou et al. (2001 ▶). For tn ligand geometry, see: Vaughn (1981 ▶). For the standard Cambridge Structural Database description, see: Allen (2002 ▶).

Experimental

Crystal data

[CrCl2(C3H10N2)2]ClO4

M = 370.61

Monoclinic,

a = 6.4306 (5) Å

b = 17.2588 (15) Å

c = 13.0235 (11) Å

β = 92.840 (4)°

V = 1443.6 (2) Å3

Z = 4

Mo Kα radiation

μ = 1.36 mm−1

T = 173 K

0.16 × 0.08 × 0.05 mm

Data collection

Bruker APEXII CCD diffractometer

Absorption correction: multi-scan (TWINABS; Sheldrick, 2008a ▶) T min = 0.815, T max = 0.930

28308 measured reflections

6269 independent reflections

5585 reflections with I > 2σ(I)

R int = 0.039

Refinement

R[F 2 > 2σ(F 2)] = 0.028

wR(F 2) = 0.075

S = 1.07

6269 reflections

245 parameters

All H-atom parameters refined

Δρmax = 0.36 e Å−3

Δρmin = −0.32 e Å−3

Data collection: APEX2 (Bruker, 2010 ▶); cell refinement: SAINT (Bruker, 2010 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008b ▶); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 2010 ▶); software used to prepare material for publication: SHELXTL and local programs.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811006349/nk2086sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811006349/nk2086Isup2.hkl

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

[CrCl2(C3H10N2)2]ClO4	F(000) = 764
Mr = 370.61	Dx = 1.705 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 6530 reflections
a = 6.4306 (5) Å	θ = 2.8–28.3°
b = 17.2588 (15) Å	µ = 1.36 mm−1
c = 13.0235 (11) Å	T = 173 K
β = 92.840 (4)°	Block, green
V = 1443.6 (2) Å3	0.16 × 0.08 × 0.05 mm
Z = 4

Bruker APEXII CCD diffractometer	6269 independent reflections
Radiation source: sealed tube	5585 reflections with I > 2σ(I)
graphite	Rint = 0.039
Thin–slice ω scans	θmax = 28.4°, θmin = 2.0°
Absorption correction: multi-scan (TWINABS; Sheldrick, 2008a)	h = −8→8
Tmin = 0.815, Tmax = 0.930	k = 0→23
28308 measured reflections	l = 0→17

Refinement on F2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028	All H-atom parameters refined
wR(F2) = 0.075	w = 1/[σ2(Fo2) + (0.0391P)2 + 1.9009P] where P = (Fo2 + 2Fc2)/3
S = 1.07	(Δ/σ)max = 0.001
6269 reflections	Δρmax = 0.36 e Å−3
245 parameters	Δρmin = −0.32 e Å−3
0 restraints	Extinction correction: SHELXTL (Sheldrick, 2008a), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0011 (6)

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
Cr	0.49360 (5)	0.396455 (18)	0.29650 (2)	0.01236 (9)
Cl1	0.24916 (7)	0.41493 (3)	0.41882 (4)	0.01906 (12)
Cl2	0.74177 (7)	0.37755 (3)	0.17627 (4)	0.01921 (12)
N1	0.7262 (3)	0.42985 (10)	0.40534 (14)	0.0149 (3)
H1A	0.840 (4)	0.4296 (16)	0.375 (2)	0.026 (7)*
H1B	0.707 (4)	0.4791 (15)	0.4214 (19)	0.015 (6)*
N2	0.5301 (3)	0.28012 (11)	0.33866 (15)	0.0177 (4)
H2A	0.619 (5)	0.2656 (17)	0.301 (2)	0.028 (8)*
H2B	0.417 (5)	0.2552 (18)	0.321 (2)	0.039 (8)*
N3	0.2572 (3)	0.36594 (12)	0.18892 (14)	0.0182 (4)
H3A	0.258 (4)	0.3159 (17)	0.182 (2)	0.027 (7)*
H3B	0.138 (5)	0.3757 (16)	0.219 (2)	0.030 (8)*
N4	0.4523 (3)	0.51159 (11)	0.25055 (15)	0.0194 (4)
H4A	0.556 (4)	0.5348 (16)	0.271 (2)	0.024 (7)*
H4B	0.356 (5)	0.5272 (16)	0.284 (2)	0.029 (8)*
C1	0.7561 (3)	0.38579 (13)	0.50303 (17)	0.0190 (4)
H1C	0.872 (4)	0.4054 (15)	0.543 (2)	0.022 (7)*
H1D	0.634 (4)	0.3944 (13)	0.5441 (19)	0.011 (6)*
C2	0.7850 (4)	0.29977 (13)	0.48554 (19)	0.0236 (5)
H2C	0.894 (4)	0.2925 (15)	0.439 (2)	0.022 (7)*
H2D	0.821 (4)	0.2755 (17)	0.550 (2)	0.034 (8)*
C3	0.5888 (4)	0.25891 (13)	0.44656 (18)	0.0222 (5)
H3C	0.605 (4)	0.2040 (16)	0.450 (2)	0.024 (7)*
H3D	0.476 (4)	0.2728 (15)	0.490 (2)	0.023 (7)*
C4	0.2446 (4)	0.40246 (14)	0.08533 (18)	0.0232 (5)
H4C	0.366 (4)	0.3889 (15)	0.051 (2)	0.022 (7)*
H4D	0.121 (4)	0.3793 (15)	0.045 (2)	0.021 (6)*
C5	0.2255 (4)	0.48944 (15)	0.09247 (19)	0.0244 (5)
H5C	0.203 (4)	0.5077 (16)	0.021 (2)	0.032 (8)*
H5D	0.104 (4)	0.5017 (16)	0.129 (2)	0.029 (7)*
C6	0.4160 (4)	0.52997 (14)	0.13932 (19)	0.0242 (5)
H6C	0.542 (4)	0.5136 (15)	0.106 (2)	0.021 (6)*
H6D	0.403 (4)	0.5848 (17)	0.135 (2)	0.029 (7)*
Cl3	0.07592 (8)	0.14746 (3)	0.25004 (4)	0.01984 (12)
O1	0.1011 (3)	0.06757 (10)	0.22292 (16)	0.0363 (4)
O2	0.1833 (3)	0.19442 (11)	0.17838 (16)	0.0384 (5)
O3	−0.1425 (3)	0.16517 (11)	0.24445 (15)	0.0358 (4)
O4	0.1632 (3)	0.16154 (14)	0.35117 (15)	0.0475 (5)

	U11	U22	U33	U12	U13	U23
Cr	0.00998 (15)	0.01357 (16)	0.01352 (17)	−0.00015 (11)	0.00047 (11)	−0.00070 (12)
Cl1	0.0142 (2)	0.0238 (3)	0.0196 (3)	0.00007 (18)	0.00468 (18)	−0.00218 (19)
Cl2	0.0131 (2)	0.0257 (3)	0.0190 (3)	0.00135 (18)	0.00347 (18)	−0.00246 (19)
N1	0.0135 (8)	0.0154 (9)	0.0160 (9)	−0.0014 (6)	0.0014 (6)	−0.0011 (7)
N2	0.0171 (8)	0.0166 (9)	0.0192 (9)	−0.0015 (7)	−0.0009 (7)	−0.0017 (7)
N3	0.0133 (8)	0.0238 (10)	0.0175 (9)	−0.0010 (7)	−0.0003 (7)	−0.0028 (7)
N4	0.0197 (9)	0.0179 (9)	0.0206 (10)	0.0006 (7)	0.0006 (8)	0.0014 (7)
C1	0.0222 (10)	0.0194 (10)	0.0150 (10)	−0.0019 (8)	−0.0024 (8)	−0.0007 (8)
C2	0.0281 (12)	0.0194 (11)	0.0226 (12)	0.0020 (9)	−0.0065 (10)	0.0011 (9)
C3	0.0310 (12)	0.0155 (10)	0.0201 (11)	−0.0035 (9)	−0.0004 (9)	0.0030 (8)
C4	0.0191 (10)	0.0338 (13)	0.0164 (11)	0.0023 (9)	−0.0017 (8)	−0.0017 (9)
C5	0.0210 (11)	0.0329 (13)	0.0193 (11)	0.0081 (9)	0.0005 (9)	0.0048 (9)
C6	0.0269 (11)	0.0243 (12)	0.0216 (11)	0.0040 (9)	0.0031 (9)	0.0080 (9)
Cl3	0.0206 (2)	0.0175 (2)	0.0210 (3)	−0.00116 (19)	−0.00290 (19)	−0.00153 (19)
O1	0.0380 (10)	0.0179 (8)	0.0530 (13)	0.0042 (7)	0.0012 (9)	−0.0030 (8)
O2	0.0452 (11)	0.0343 (10)	0.0364 (11)	−0.0138 (9)	0.0092 (9)	0.0050 (8)
O3	0.0246 (9)	0.0394 (10)	0.0434 (12)	0.0087 (8)	0.0019 (8)	−0.0052 (9)
O4	0.0523 (13)	0.0653 (15)	0.0235 (10)	−0.0131 (11)	−0.0121 (9)	−0.0053 (10)

Cr—Cl1	2.3148 (6)	C1—H1D	0.98 (2)
Cr—Cl2	2.3135 (6)	C1—C2	1.515 (3)
Cr—N1	2.0903 (18)	C2—H2C	0.95 (3)
Cr—N2	2.0917 (19)	C2—H2D	0.96 (3)
Cr—N3	2.0831 (18)	C2—C3	1.511 (3)
Cr—N4	2.0884 (19)	C3—H3C	0.95 (3)
N1—H1A	0.85 (3)	C3—H3D	0.97 (3)
N1—H1B	0.89 (3)	C4—H4C	0.95 (3)
N1—C1	1.486 (3)	C4—H4D	1.02 (3)
N2—H2A	0.81 (3)	C4—C5	1.510 (3)
N2—H2B	0.86 (3)	C5—H5C	0.99 (3)
N2—C3	1.483 (3)	C5—H5D	0.95 (3)
N3—H3A	0.87 (3)	C5—C6	1.513 (3)
N3—H3B	0.89 (3)	C6—H6C	0.98 (3)
N3—C4	1.488 (3)	C6—H6D	0.95 (3)
N4—H4A	0.81 (3)	Cl3—O1	1.4346 (18)
N4—H4B	0.82 (3)	Cl3—O2	1.4380 (19)
N4—C6	1.490 (3)	Cl3—O3	1.4360 (18)
C1—H1C	0.95 (3)	Cl3—O4	1.4268 (19)
Cl1—Cr—Cl2	179.11 (2)	N1—C1—C2	112.60 (19)
Cl1—Cr—N1	89.02 (5)	H1C—C1—H1D	106 (2)
Cl1—Cr—N2	91.31 (6)	H1C—C1—C2	109.5 (15)
Cl1—Cr—N3	90.00 (6)	H1D—C1—C2	109.7 (13)
Cl1—Cr—N4	89.14 (6)	C1—C2—H2C	108.8 (16)
Cl2—Cr—N1	90.19 (5)	C1—C2—H2D	108.8 (18)
Cl2—Cr—N2	88.28 (6)	C1—C2—C3	113.6 (2)
Cl2—Cr—N3	90.80 (6)	H2C—C2—H2D	110 (2)
Cl2—Cr—N4	91.29 (6)	H2C—C2—C3	110.8 (16)
N1—Cr—N2	91.11 (7)	H2D—C2—C3	104.7 (17)
N1—Cr—N3	178.42 (8)	N2—C3—C2	111.85 (19)
N1—Cr—N4	90.49 (7)	N2—C3—H3C	108.4 (16)
N2—Cr—N3	90.15 (8)	N2—C3—H3D	108.9 (16)
N2—Cr—N4	178.34 (8)	C2—C3—H3C	111.0 (16)
N3—Cr—N4	88.26 (8)	C2—C3—H3D	109.1 (16)
Cr—N1—H1A	106.5 (19)	H3C—C3—H3D	107 (2)
Cr—N1—H1B	108.7 (16)	N3—C4—H4C	108.4 (16)
Cr—N1—C1	119.81 (13)	N3—C4—H4D	108.1 (15)
H1A—N1—H1B	104 (2)	N3—C4—C5	111.49 (19)
H1A—N1—C1	108.7 (19)	H4C—C4—H4D	107 (2)
H1B—N1—C1	107.6 (16)	H4C—C4—C5	110.2 (16)
Cr—N2—H2A	102 (2)	H4D—C4—C5	111.1 (14)
Cr—N2—H2B	109 (2)	C4—C5—H5C	105.6 (16)
Cr—N2—C3	120.38 (14)	C4—C5—H5D	108.8 (17)
H2A—N2—H2B	107 (3)	C4—C5—C6	114.71 (19)
H2A—N2—C3	110 (2)	H5C—C5—H5D	108 (2)
H2B—N2—C3	108 (2)	H5C—C5—C6	108.0 (16)
Cr—N3—H3A	108.3 (19)	H5D—C5—C6	111.2 (17)
Cr—N3—H3B	105.8 (19)	N4—C6—C5	112.24 (19)
Cr—N3—C4	120.53 (14)	N4—C6—H6C	106.3 (15)
H3A—N3—H3B	104 (3)	N4—C6—H6D	106.0 (17)
H3A—N3—C4	109.2 (19)	C5—C6—H6C	110.9 (15)
H3B—N3—C4	107.9 (19)	C5—C6—H6D	111.8 (17)
Cr—N4—H4A	107 (2)	H6C—C6—H6D	109 (2)
Cr—N4—H4B	104 (2)	O1—Cl3—O2	108.55 (12)
Cr—N4—C6	119.53 (15)	O1—Cl3—O3	108.32 (11)
H4A—N4—H4B	107 (3)	O1—Cl3—O4	110.29 (13)
H4A—N4—C6	108 (2)	O2—Cl3—O3	110.30 (12)
H4B—N4—C6	111 (2)	O2—Cl3—O4	108.88 (13)
N1—C1—H1C	110.3 (16)	O3—Cl3—O4	110.48 (13)
N1—C1—H1D	108.4 (14)
Cl1—Cr—N1—C1	59.00 (15)	Cl1—Cr—N4—C6	−130.76 (17)
Cl2—Cr—N1—C1	−120.57 (15)	Cl2—Cr—N4—C6	50.02 (17)
N2—Cr—N1—C1	−32.28 (16)	N1—Cr—N4—C6	140.22 (17)
N4—Cr—N1—C1	148.14 (16)	N3—Cr—N4—C6	−40.74 (17)
Cl1—Cr—N2—C3	−56.16 (16)	Cr—N1—C1—C2	53.7 (2)
Cl2—Cr—N2—C3	123.04 (16)	N1—C1—C2—C3	−71.2 (3)
N1—Cr—N2—C3	32.88 (17)	Cr—N2—C3—C2	−54.3 (2)
N3—Cr—N2—C3	−146.17 (17)	C1—C2—C3—N2	71.1 (3)
Cl1—Cr—N3—C4	130.33 (16)	Cr—N3—C4—C5	−58.4 (2)
Cl2—Cr—N3—C4	−50.08 (16)	N3—C4—C5—C6	67.0 (3)
N2—Cr—N3—C4	−138.36 (17)	Cr—N4—C6—C5	58.4 (2)
N4—Cr—N3—C4	41.19 (17)	C4—C5—C6—N4	−67.7 (3)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···Cl1i	0.85 (3)	2.68 (3)	3.3684 (19)	139 (2)
N1—H1B···Cl1ii	0.89 (3)	2.77 (3)	3.5229 (19)	143 (2)
N2—H2A···O3i	0.81 (3)	2.45 (3)	3.182 (3)	151 (3)
N2—H2A···Cl2	0.81 (3)	2.67 (3)	3.072 (2)	112 (2)
N2—H2B···O4	0.86 (3)	2.35 (3)	3.134 (3)	151 (3)
N2—H2B···O2	0.86 (3)	2.56 (3)	3.326 (3)	149 (3)
N3—H3A···O2	0.87 (3)	2.15 (3)	3.000 (3)	166 (3)
N3—H3B···Cl2iii	0.89 (3)	2.58 (3)	3.3168 (19)	140 (2)
N4—H4A···O1iv	0.81 (3)	2.28 (3)	3.033 (3)	156 (3)

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯Cl1i	0.85 (3)	2.68 (3)	3.3684 (19)	139 (2)
N1—H1B⋯Cl1ii	0.89 (3)	2.77 (3)	3.5229 (19)	143 (2)
N2—H2A⋯O3i	0.81 (3)	2.45 (3)	3.182 (3)	151 (3)
N2—H2A⋯Cl2	0.81 (3)	2.67 (3)	3.072 (2)	112 (2)
N2—H2B⋯O4	0.86 (3)	2.35 (3)	3.134 (3)	151 (3)
N2—H2B⋯O2	0.86 (3)	2.56 (3)	3.326 (3)	149 (3)
N3—H3A⋯O2	0.87 (3)	2.15 (3)	3.000 (3)	166 (3)
N3—H3B⋯Cl2iii	0.89 (3)	2.58 (3)	3.3168 (19)	140 (2)
N4—H4A⋯O1iv	0.81 (3)	2.28 (3)	3.033 (3)	156 (3)

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