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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Volume 67| Part 3| March 2011| Page m381
doi:10.1107/S1600536811006349

trans-Di­chloridobis(propane-1,3-di­amine-κ2N,N′)chromium(III) perchlorate

Jong-Ha Choia and William Cleggb*

aDepartment of Chemistry, Andong National University, Andong 760-749, Republic of Korea, and bSchool of Chemistry, Newcastle University, Newcastle upon Tyne NE1 7RU, England
*Correspondence e-mail: w.clegg@ncl.ac.uk

(Received 7 February 2011; accepted 19 February 2011; online 26 February 2011)

In the title compound, [CrCl2(C3H10N2)2]ClO4, the CrIII 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 octa­hedral 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 tetra­hedral geometries. Weak inter­molecular 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[Couldwell, M. C. & House, D. A. (1972). Inorg. Chem. 11, 2024-2031.]); House (1970[House, D. A. (1970). Inorg. Nucl. Chem. Lett. 6, 741-746.]). For related structures, see: Choi et al. (2002[Choi, J.-H., Suzuki, T. & Kaizaki, S. (2002). Acta Cryst. C58, m539-m541.], 2007[Choi, J. H., Clegg, W., Nichol, G. S., Lee, S. H., Park, Y. C. & Habibi, M. H. (2007). Spectrochim. Acta Part A, 68, 796-801.], 2008[Choi, J.-H., Lee, S. H. & Lee, U. (2008). Acta Cryst. E64, m1429.], 2010[Choi, J. H., Clegg, W., Harrington, R. W. & Lee, S. H. (2010). J. Chem. Crystallogr. 40, 567-571.]); Vaughn & Rogers (1985[Vaughn, J. W. & Rogers, R. D. (1985). J. Crystallogr. Spectrosc. Res. 15, 281-287.]); Kou et al. (2001[Kou, H.-Z., Gao, D.-Z., Bu, W.-M., Fan, Y.-G., Liao, D.-Z., Cheng, P., Jiang, Z.-H., Yan, S.-P., Wang, G.-L., Li, T.-J. & Tang, J.-K. (2001). Transition Met. Chem. 26, 457-460.]). For tn ligand geometry, see: Vaughn (1981[Vaughn, J. W. (1981). Inorg. Chem. 20, 2397-2402.]). For the standard Cambridge Structural Database description, see: Allen (2002[Allen, F. H. (2002). Acta Cryst. B58, 380-388.]).

[Scheme 1]

Experimental

Crystal data

  • [CrCl2(C3H10N2)2]ClO4

  • Mr = 370.61

  • Monoclinic, P 21 /c

  • 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[Sheldrick, G. M. (2008a). TWINABS. University of Göttingen, Germany.]) Tmin = 0.815, Tmax = 0.930

  • 28308 measured reflections

  • 6269 independent reflections

  • 5585 reflections with I > 2σ(I)

  • Rint = 0.039
Refinement

  • R[F2 > 2σ(F2)] = 0.028

  • wR(F2) = 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

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) x+1, y, z; (ii) -x+1, -y+1, -z+1; (iii) x-1, y, z; (iv) [-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}].

Data collection: APEX2 (Bruker, 2010[Bruker (2010). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2010[Bruker (2010). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008b[Sheldrick, G. M. (2008b). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXTL; molecular graphics: DIAMOND (Brandenburg, 2010[Brandenburg, K. (2010). DIAMOND. Crystal Impact GbR, Bonn, Germany.]); software used to prepare material for publication: SHELXTL and local programs.

Supporting information

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

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

checkCIF report


Comment top

The [Cr(tn)2L2]+ cation (tn = propane-1,3-diamine, L = monodentate ligand) can exist as trans and cis geometric isomers. There are also two possible conformations with respect to the six-membered chelate rings (present as chairs) in the trans geometric isomer: the carbon atoms of these rings in the two tn ligands can be located on the same side (syn conformer) or on opposite side (anti conformer) of the equatorial plane. In the crystal structures of trans-[Cr(Me2tn)2Cl2]Cl and trans-[Cr(Me2tn)2Br2]2Br2.HClO4.6H2O (Me2tn = 2,2-dimethylpropane-1,3-diamine), both syn and anti conformational isomers are found together (Choi et al., 2002; Choi et al., 2007), while trans-[Cr(Me2tn)2Cl2]ClO4 (Choi et al., 2008) has only the anti conformer, as do trans-[Cr(tn)2F2]ClO4 (Vaughn & Rogers, 1985) and trans-[Cr(tn)2Cl2]3[Fe(CN)6.6H2O (Kou et al., 2001). The preference for syn or anti conformation of chelate rings in trans complex cations with tn or Me2tn ligands is thus subtle and worthy of further study. Infrared and electronic absorption spectroscopic methods are not useful in distinguishing such syn and anti conformations in these metal complexes. Structural studies of bromido-containing chromium(III) complexes are relatively rare compared to those with chlorido ligands. Therefore we attempted to prepare trans-[Cr(tn)2Br2]ClO4 by a literature method (Couldwell & House, 1972); its UV-visible and IR spectra are nearly the same as those of trans-[Cr(tn)2Cl2]ClO4 (House, 1970), and it was only with a crystal structure analysis that we established that the product was actually the dichlorido rather than the dibromido complex. We report here the structure of trans-[Cr(tn)2Cl2]ClO4 (I) which provides further information on the conformation of the two six-membered chelate rings.

In the title complex (I), the chromium(III) ion is coplanar with the four coordinating N atoms and adopts an octahedral geometry, in which the four nitrogen atoms of two tn ligands occupy the equatorial sites and the two chlorine atoms coordinate axially in a trans configuration. The two six-membered rings have their usual stable chair conformations, and they are exclusively in the anti conformation with respect to each other in the unique cation of the asymmetric unit (Fig. 1).

The Cr—N distances (Table 1) are in the range 2.0831 (18)–2.0917 (19) Å, typical for Cr—N bonds involving primary amines (Choi et al., 2002; Choi et al., 2007). The Cr—Cl distances [2.3135 (6) and 2.3148 (6) Å] are very close to the values 2.3179 (9) and 2.3212 (4) Å found in trans-[Cr(Me2tn)2Cl2]ClO4 (Choi et al., 2008), and typical generally of Cr—Cl bond lengths in the Cambridge Structural Database (Allen, 2002), but shorter than the 2.4743 (10) Å for Cr—Br bond lengths in trans-[Cr(en)2Br2]ClO4 (Choi et al., 2010). The assignment of the axial ligands as Cl rather than the Br intended and expected from the synthesis is also clearly correct from the satisfactory refinement of anisotropic displacement parameters, demonstrating an appropriate electron density. The internal geometry of the tn ligands is typical for these in chair conformations (Vaughn, 1981). The uncoordinated ClO4- anion shows an essentially tetrahedral arrangement with Cl—O distances in the range 1.4268 (19)–1.4380 (19) Å and the angles at Cl ranging from 108.32 (11) to 110.48 (13)°. There is an extensive weak hydrogen bonding network involving the oxygen atoms of the anions, chlorido ligands, and the N—H groups of the tn ligands (Table 2), which supports the main ionic interactions in this complex salt.

Related literature top

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 top

The ligand propane-1,3-diamine was obtained from Aldrich Chemical Co. and was used as supplied. All other chemicals were reagent grade materials and were used without further purification. We intended to prepare trans-[Cr(tn)2Br2]ClO4 as described in the literature (Couldwell & House, 1972) but obtained instead trans-[Cr(tn)2Cl2]ClO4, as demonstrated by this crystal structure analysis.

CrCl3.6H2O (5.4 g) was dissolved in DMSO (25 ml) and the solution was boiled for 10 min. A mixture of 1,3-propanediamine (3 ml) and DMSO (15 ml) was added and boiling was continued for 2 min. After cooling to 60°C, the solution was poured into well stirred acetone (300 ml). The precipitate was filtered off and washed with acetone, then dissolved in aqueous HBr (20 ml, 48%) and the solution was heated on a steam bath for 15 min. and filtered. The filtrate was heated on a steam bath for a further 15 min. Aqueous HClO4 (5 ml, 60%) was added to the solution. The resulting green crystals were collected and washed with ethanol. The infrared spectrum (nujol) was consistent with the crystallographically determined structure. The chloro ligands in the title compound are clearly retained from the chromium(III) chloride starting material, and were not substituted as intended by Br in the reaction with HBr.

Refinement top

The crystal was a non-merohedral twin with a 23.45 (6)% contribution of the minor component according to the refinement; because of the twinning, merging of symmetry-equivalent data could not be performed prior to refinement. The twin law is 1 0 0 / 0 - 1 0 / -0.2 0 - 1, corresponding to a 180° rotation about the a axis. Hydrogen atoms were located in a difference map and refined freely with individual isotropic displacement parameters.

Computing details top

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

Figures top
[Figure 1] Fig. 1. The structure of the complex cation and anion (displacement ellipsoids are drawn at the 50% probability level).
trans-Dichloridobis(propane-1,3-diamine- κ2N,N')chromium(III) perchlorate top
Crystal data top
[CrCl2(C3H10N2)2]ClO4F(000) = 764
Mr = 370.61Dx = 1.705 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 6530 reflections
a = 6.4306 (5) Åθ = 2.8–28.3°
b = 17.2588 (15) ŵ = 1.36 mm−1
c = 13.0235 (11) ÅT = 173 K
β = 92.840 (4)°Block, green
V = 1443.6 (2) Å30.16 × 0.08 × 0.05 mm
Z = 4
Data collection top
Bruker APEXII CCD
diffractometer		6269 independent reflections
Radiation source: sealed tube5585 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.039
Thin–slice ω scansθmax = 28.4°, θmin = 2.0°
Absorption correction: multi-scan
(TWINABS; Sheldrick, 2008a)		h = −8→8
Tmin = 0.815, Tmax = 0.930k = 0→23
28308 measured reflectionsl = 0→17
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.028All 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 reflectionsΔρmax = 0.36 e Å−3
245 parametersΔρmin = −0.32 e Å−3
0 restraintsExtinction correction: SHELXTL (Sheldrick, 2008a), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0011 (6)
Crystal data top
[CrCl2(C3H10N2)2]ClO4V = 1443.6 (2) Å3
Mr = 370.61Z = 4
Monoclinic, P21/cMo Kα radiation
a = 6.4306 (5) ŵ = 1.36 mm−1
b = 17.2588 (15) ÅT = 173 K
c = 13.0235 (11) Å0.16 × 0.08 × 0.05 mm
β = 92.840 (4)°
Data collection top
Bruker APEXII CCD
diffractometer		6269 independent reflections
Absorption correction: multi-scan
(TWINABS; Sheldrick, 2008a)		5585 reflections with I > 2σ(I)
Tmin = 0.815, Tmax = 0.930Rint = 0.039
28308 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0280 restraints
wR(F2) = 0.075All H-atom parameters refined
S = 1.07Δρmax = 0.36 e Å−3
6269 reflectionsΔρmin = −0.32 e Å−3
245 parameters
Special details top

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 (Å2) top
xyzUiso*/Ueq
Cr0.49360 (5)0.396455 (18)0.29650 (2)0.01236 (9)
Cl10.24916 (7)0.41493 (3)0.41882 (4)0.01906 (12)
Cl20.74177 (7)0.37755 (3)0.17627 (4)0.01921 (12)
N10.7262 (3)0.42985 (10)0.40534 (14)0.0149 (3)
H1A0.840 (4)0.4296 (16)0.375 (2)0.026 (7)*
H1B0.707 (4)0.4791 (15)0.4214 (19)0.015 (6)*
N20.5301 (3)0.28012 (11)0.33866 (15)0.0177 (4)
H2A0.619 (5)0.2656 (17)0.301 (2)0.028 (8)*
H2B0.417 (5)0.2552 (18)0.321 (2)0.039 (8)*
N30.2572 (3)0.36594 (12)0.18892 (14)0.0182 (4)
H3A0.258 (4)0.3159 (17)0.182 (2)0.027 (7)*
H3B0.138 (5)0.3757 (16)0.219 (2)0.030 (8)*
N40.4523 (3)0.51159 (11)0.25055 (15)0.0194 (4)
H4A0.556 (4)0.5348 (16)0.271 (2)0.024 (7)*
H4B0.356 (5)0.5272 (16)0.284 (2)0.029 (8)*
C10.7561 (3)0.38579 (13)0.50303 (17)0.0190 (4)
H1C0.872 (4)0.4054 (15)0.543 (2)0.022 (7)*
H1D0.634 (4)0.3944 (13)0.5441 (19)0.011 (6)*
C20.7850 (4)0.29977 (13)0.48554 (19)0.0236 (5)
H2C0.894 (4)0.2925 (15)0.439 (2)0.022 (7)*
H2D0.821 (4)0.2755 (17)0.550 (2)0.034 (8)*
C30.5888 (4)0.25891 (13)0.44656 (18)0.0222 (5)
H3C0.605 (4)0.2040 (16)0.450 (2)0.024 (7)*
H3D0.476 (4)0.2728 (15)0.490 (2)0.023 (7)*
C40.2446 (4)0.40246 (14)0.08533 (18)0.0232 (5)
H4C0.366 (4)0.3889 (15)0.051 (2)0.022 (7)*
H4D0.121 (4)0.3793 (15)0.045 (2)0.021 (6)*
C50.2255 (4)0.48944 (15)0.09247 (19)0.0244 (5)
H5C0.203 (4)0.5077 (16)0.021 (2)0.032 (8)*
H5D0.104 (4)0.5017 (16)0.129 (2)0.029 (7)*
C60.4160 (4)0.52997 (14)0.13932 (19)0.0242 (5)
H6C0.542 (4)0.5136 (15)0.106 (2)0.021 (6)*
H6D0.403 (4)0.5848 (17)0.135 (2)0.029 (7)*
Cl30.07592 (8)0.14746 (3)0.25004 (4)0.01984 (12)
O10.1011 (3)0.06757 (10)0.22292 (16)0.0363 (4)
O20.1833 (3)0.19442 (11)0.17838 (16)0.0384 (5)
O3−0.1425 (3)0.16517 (11)0.24445 (15)0.0358 (4)
O40.1632 (3)0.16154 (14)0.35117 (15)0.0475 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr0.00998 (15)0.01357 (16)0.01352 (17)−0.00015 (11)0.00047 (11)−0.00070 (12)
Cl10.0142 (2)0.0238 (3)0.0196 (3)0.00007 (18)0.00468 (18)−0.00218 (19)
Cl20.0131 (2)0.0257 (3)0.0190 (3)0.00135 (18)0.00347 (18)−0.00246 (19)
N10.0135 (8)0.0154 (9)0.0160 (9)−0.0014 (6)0.0014 (6)−0.0011 (7)
N20.0171 (8)0.0166 (9)0.0192 (9)−0.0015 (7)−0.0009 (7)−0.0017 (7)
N30.0133 (8)0.0238 (10)0.0175 (9)−0.0010 (7)−0.0003 (7)−0.0028 (7)
N40.0197 (9)0.0179 (9)0.0206 (10)0.0006 (7)0.0006 (8)0.0014 (7)
C10.0222 (10)0.0194 (10)0.0150 (10)−0.0019 (8)−0.0024 (8)−0.0007 (8)
C20.0281 (12)0.0194 (11)0.0226 (12)0.0020 (9)−0.0065 (10)0.0011 (9)
C30.0310 (12)0.0155 (10)0.0201 (11)−0.0035 (9)−0.0004 (9)0.0030 (8)
C40.0191 (10)0.0338 (13)0.0164 (11)0.0023 (9)−0.0017 (8)−0.0017 (9)
C50.0210 (11)0.0329 (13)0.0193 (11)0.0081 (9)0.0005 (9)0.0048 (9)
C60.0269 (11)0.0243 (12)0.0216 (11)0.0040 (9)0.0031 (9)0.0080 (9)
Cl30.0206 (2)0.0175 (2)0.0210 (3)−0.00116 (19)−0.00290 (19)−0.00153 (19)
O10.0380 (10)0.0179 (8)0.0530 (13)0.0042 (7)0.0012 (9)−0.0030 (8)
O20.0452 (11)0.0343 (10)0.0364 (11)−0.0138 (9)0.0092 (9)0.0050 (8)
O30.0246 (9)0.0394 (10)0.0434 (12)0.0087 (8)0.0019 (8)−0.0052 (9)
O40.0523 (13)0.0653 (15)0.0235 (10)−0.0131 (11)−0.0121 (9)−0.0053 (10)
Geometric parameters (Å, º) top
Cr—Cl12.3148 (6)C1—H1D0.98 (2)
Cr—Cl22.3135 (6)C1—C21.515 (3)
Cr—N12.0903 (18)C2—H2C0.95 (3)
Cr—N22.0917 (19)C2—H2D0.96 (3)
Cr—N32.0831 (18)C2—C31.511 (3)
Cr—N42.0884 (19)C3—H3C0.95 (3)
N1—H1A0.85 (3)C3—H3D0.97 (3)
N1—H1B0.89 (3)C4—H4C0.95 (3)
N1—C11.486 (3)C4—H4D1.02 (3)
N2—H2A0.81 (3)C4—C51.510 (3)
N2—H2B0.86 (3)C5—H5C0.99 (3)
N2—C31.483 (3)C5—H5D0.95 (3)
N3—H3A0.87 (3)C5—C61.513 (3)
N3—H3B0.89 (3)C6—H6C0.98 (3)
N3—C41.488 (3)C6—H6D0.95 (3)
N4—H4A0.81 (3)Cl3—O11.4346 (18)
N4—H4B0.82 (3)Cl3—O21.4380 (19)
N4—C61.490 (3)Cl3—O31.4360 (18)
C1—H1C0.95 (3)Cl3—O41.4268 (19)
Cl1—Cr—Cl2179.11 (2)N1—C1—C2112.60 (19)
Cl1—Cr—N189.02 (5)H1C—C1—H1D106 (2)
Cl1—Cr—N291.31 (6)H1C—C1—C2109.5 (15)
Cl1—Cr—N390.00 (6)H1D—C1—C2109.7 (13)
Cl1—Cr—N489.14 (6)C1—C2—H2C108.8 (16)
Cl2—Cr—N190.19 (5)C1—C2—H2D108.8 (18)
Cl2—Cr—N288.28 (6)C1—C2—C3113.6 (2)
Cl2—Cr—N390.80 (6)H2C—C2—H2D110 (2)
Cl2—Cr—N491.29 (6)H2C—C2—C3110.8 (16)
N1—Cr—N291.11 (7)H2D—C2—C3104.7 (17)
N1—Cr—N3178.42 (8)N2—C3—C2111.85 (19)
N1—Cr—N490.49 (7)N2—C3—H3C108.4 (16)
N2—Cr—N390.15 (8)N2—C3—H3D108.9 (16)
N2—Cr—N4178.34 (8)C2—C3—H3C111.0 (16)
N3—Cr—N488.26 (8)C2—C3—H3D109.1 (16)
Cr—N1—H1A106.5 (19)H3C—C3—H3D107 (2)
Cr—N1—H1B108.7 (16)N3—C4—H4C108.4 (16)
Cr—N1—C1119.81 (13)N3—C4—H4D108.1 (15)
H1A—N1—H1B104 (2)N3—C4—C5111.49 (19)
H1A—N1—C1108.7 (19)H4C—C4—H4D107 (2)
H1B—N1—C1107.6 (16)H4C—C4—C5110.2 (16)
Cr—N2—H2A102 (2)H4D—C4—C5111.1 (14)
Cr—N2—H2B109 (2)C4—C5—H5C105.6 (16)
Cr—N2—C3120.38 (14)C4—C5—H5D108.8 (17)
H2A—N2—H2B107 (3)C4—C5—C6114.71 (19)
H2A—N2—C3110 (2)H5C—C5—H5D108 (2)
H2B—N2—C3108 (2)H5C—C5—C6108.0 (16)
Cr—N3—H3A108.3 (19)H5D—C5—C6111.2 (17)
Cr—N3—H3B105.8 (19)N4—C6—C5112.24 (19)
Cr—N3—C4120.53 (14)N4—C6—H6C106.3 (15)
H3A—N3—H3B104 (3)N4—C6—H6D106.0 (17)
H3A—N3—C4109.2 (19)C5—C6—H6C110.9 (15)
H3B—N3—C4107.9 (19)C5—C6—H6D111.8 (17)
Cr—N4—H4A107 (2)H6C—C6—H6D109 (2)
Cr—N4—H4B104 (2)O1—Cl3—O2108.55 (12)
Cr—N4—C6119.53 (15)O1—Cl3—O3108.32 (11)
H4A—N4—H4B107 (3)O1—Cl3—O4110.29 (13)
H4A—N4—C6108 (2)O2—Cl3—O3110.30 (12)
H4B—N4—C6111 (2)O2—Cl3—O4108.88 (13)
N1—C1—H1C110.3 (16)O3—Cl3—O4110.48 (13)
N1—C1—H1D108.4 (14)
Cl1—Cr—N1—C159.00 (15)Cl1—Cr—N4—C6−130.76 (17)
Cl2—Cr—N1—C1−120.57 (15)Cl2—Cr—N4—C650.02 (17)
N2—Cr—N1—C1−32.28 (16)N1—Cr—N4—C6140.22 (17)
N4—Cr—N1—C1148.14 (16)N3—Cr—N4—C6−40.74 (17)
Cl1—Cr—N2—C3−56.16 (16)Cr—N1—C1—C253.7 (2)
Cl2—Cr—N2—C3123.04 (16)N1—C1—C2—C3−71.2 (3)
N1—Cr—N2—C332.88 (17)Cr—N2—C3—C2−54.3 (2)
N3—Cr—N2—C3−146.17 (17)C1—C2—C3—N271.1 (3)
Cl1—Cr—N3—C4130.33 (16)Cr—N3—C4—C5−58.4 (2)
Cl2—Cr—N3—C4−50.08 (16)N3—C4—C5—C667.0 (3)
N2—Cr—N3—C4−138.36 (17)Cr—N4—C6—C558.4 (2)
N4—Cr—N3—C441.19 (17)C4—C5—C6—N4−67.7 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···Cl1i0.85 (3)2.68 (3)3.3684 (19)139 (2)
N1—H1B···Cl1ii0.89 (3)2.77 (3)3.5229 (19)143 (2)
N2—H2A···O3i0.81 (3)2.45 (3)3.182 (3)151 (3)
N2—H2A···Cl20.81 (3)2.67 (3)3.072 (2)112 (2)
N2—H2B···O40.86 (3)2.35 (3)3.134 (3)151 (3)
N2—H2B···O20.86 (3)2.56 (3)3.326 (3)149 (3)
N3—H3A···O20.87 (3)2.15 (3)3.000 (3)166 (3)
N3—H3B···Cl2iii0.89 (3)2.58 (3)3.3168 (19)140 (2)
N4—H4A···O1iv0.81 (3)2.28 (3)3.033 (3)156 (3)
Symmetry codes: (i) x+1, y, z; (ii) −x+1, −y+1, −z+1; (iii) x−1, y, z; (iv) −x+1, y+1/2, −z+1/2.

Experimental details

Crystal data
Chemical formula[CrCl2(C3H10N2)2]ClO4
Mr370.61
Crystal system, space groupMonoclinic, P21/c
Temperature (K)173
a, b, c (Å)6.4306 (5), 17.2588 (15), 13.0235 (11)
β (°) 92.840 (4)
V (Å3)1443.6 (2)
Z4
Radiation typeMo Kα
µ (mm−1)1.36
Crystal size (mm)0.16 × 0.08 × 0.05
Data collection
DiffractometerBruker APEXII CCD
diffractometer
Absorption correctionMulti-scan
(TWINABS; Sheldrick, 2008a)
Tmin, Tmax0.815, 0.930
No. of measured, independent and
observed [I > 2σ(I)] reflections		28308, 6269, 5585
Rint0.039
(sin θ/λ)max (Å−1)0.669
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.028, 0.075, 1.07
No. of reflections6269
No. of parameters245
H-atom treatmentAll H-atom parameters refined
Δρmax, Δρmin (e Å−3)0.36, −0.32

Computer programs: APEX2 (Bruker, 2010), SAINT (Bruker, 2010), DIAMOND (Brandenburg, 2010), SHELXTL (Sheldrick, 2008b) and local programs.

Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···Cl1i0.85 (3)2.68 (3)3.3684 (19)139 (2)
N1—H1B···Cl1ii0.89 (3)2.77 (3)3.5229 (19)143 (2)
N2—H2A···O3i0.81 (3)2.45 (3)3.182 (3)151 (3)
N2—H2A···Cl20.81 (3)2.67 (3)3.072 (2)112 (2)
N2—H2B···O40.86 (3)2.35 (3)3.134 (3)151 (3)
N2—H2B···O20.86 (3)2.56 (3)3.326 (3)149 (3)
N3—H3A···O20.87 (3)2.15 (3)3.000 (3)166 (3)
N3—H3B···Cl2iii0.89 (3)2.58 (3)3.3168 (19)140 (2)
N4—H4A···O1iv0.81 (3)2.28 (3)3.033 (3)156 (3)
Symmetry codes: (i) x+1, y, z; (ii) −x+1, −y+1, −z+1; (iii) x−1, y, z; (iv) −x+1, y+1/2, −z+1/2.
 

Acknowledgements

This work was supported by a grant from the 2010 Research Fund of Andong National University.

References

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ISSN: 2056-9890
Volume 67| Part 3| March 2011| Page m381
doi:10.1107/S1600536811006349
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