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In the structure of the title compound, [CoCl2(C10H24N4)]Cl, the CoIII atom has a six-coordinate arrangement displaying distorted octa­hedral coordination geometry with the four N atoms from the 1,4,8,11-tetra­azacyclo­tetra­decane ring in the equatorial plane and two chloride anions in axial positions. The Co atom is located on a centre of inversion; the two Cl ions not bonded to Co are located on special positions of site symmetry \overline{4}.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806021830/bt2100sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806021830/bt2100Isup2.hkl
Contains datablock I

CCDC reference: 613591

Key indicators

  • Single-crystal X-ray study
  • T = 95 K
  • Mean [sigma](C-C) = 0.002 Å
  • R factor = 0.020
  • wR factor = 0.056
  • Data-to-parameter ratio = 12.9

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving . ?
Alert level C PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 10 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 10 C5 -N1 -CO1 -N1 41.13 0.14 5.665 1.555 1.555 5.665 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 11 C1 -N1 -CO1 -N1 168.90 0.12 1.555 1.555 1.555 5.665 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 24 C2 -N2 -CO1 -N2 1.00 0.00 1.555 1.555 1.555 5.665 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 25 C3 -N2 -CO1 -N2 14.00 0.00 1.555 1.555 1.555 5.665
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 6 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis CCD; data reduction: CrysAlis CCD [or RED?]; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997, 2005); software used to prepare material for publication: SHELXL97.

trans-Dichloro(1,4,8,11-tetraazacyclotetradecane)cobalt(III) chloride top
Crystal data top
[CoCl2(C10H24N4)]ClDx = 1.618 Mg m3
Mr = 365.61Mo Kα radiation, λ = 0.71073 Å
Tetragonal, P42/nCell parameters from 2744 reflections
a = 10.610 (1) Åθ = 2.7–26.9°
c = 13.335 (1) ŵ = 1.67 mm1
V = 1501.1 (2) Å3T = 95 K
Z = 4Prism, green
F(000) = 7600.36 × 0.28 × 0.14 mm
Data collection top
Oxford Diffraction Xcalibur
diffractometer
1535 independent reflections
Radiation source: fine-focus sealed tube1156 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.021
Rotation method data acquisition using ω and φ scansθmax = 26.4°, θmin = 2.5°
Absorption correction: analytical
(CrysAlis RED; Oxford Diffraction, 2004)
h = 139
Tmin = 0.585, Tmax = 0.800k = 1313
10515 measured reflectionsl = 1616
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.020Hydrogen site location: difference Fourier map
wR(F2) = 0.057Only H-atom coordinates refined
S = 1.05 w = 1/[σ2(Fo2) + (0.0348P)2]
where P = (Fo2 + 2Fc2)/3
1535 reflections(Δ/σ)max = 0.002
119 parametersΔρmax = 0.31 e Å3
0 restraintsΔρmin = 0.26 e Å3
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
C10.51742 (15)0.46078 (16)0.20743 (11)0.0152 (3)
H1A0.6083 (15)0.4596 (14)0.2085 (11)0.018*
H1B0.4783 (13)0.4244 (14)0.2706 (11)0.018*
C20.47445 (15)0.59485 (15)0.19531 (11)0.0157 (3)
H2A0.3879 (14)0.6003 (14)0.1914 (11)0.019*
H2B0.5070 (14)0.6487 (14)0.2506 (11)0.019*
C30.47571 (16)0.76665 (14)0.07298 (12)0.0172 (3)
H3A0.5018 (14)0.8252 (14)0.1251 (12)0.021*
H3B0.3838 (15)0.7641 (13)0.0739 (11)0.021*
C40.52161 (16)0.81297 (15)0.02826 (12)0.0172 (4)
H4A0.6142 (16)0.8177 (14)0.0343 (11)0.021*
H4B0.4948 (14)0.9002 (16)0.0368 (11)0.021*
C50.47110 (15)0.73829 (14)0.11579 (12)0.0157 (3)
H5A0.4950 (14)0.7781 (14)0.1785 (12)0.019*
H5B0.3823 (14)0.7289 (13)0.1122 (11)0.019*
N10.47542 (11)0.39036 (11)0.11758 (9)0.0121 (3)
H1C0.3962 (14)0.3826 (14)0.1230 (10)0.015*
N20.52346 (11)0.63880 (11)0.09730 (9)0.0126 (3)
H2C0.5987 (15)0.6472 (14)0.1032 (11)0.015*
Cl10.29000 (3)0.53134 (3)0.00347 (2)0.01341 (12)
Cl20.25000.25000.25000.01473 (17)
Cl30.75000.75000.25000.01723 (18)
Co10.50000.50000.00000.00843 (11)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0149 (8)0.0210 (8)0.0097 (8)0.0031 (6)0.0006 (6)0.0008 (7)
C20.0162 (8)0.0199 (9)0.0111 (7)0.0033 (7)0.0026 (7)0.0030 (7)
C30.0186 (9)0.0118 (8)0.0212 (9)0.0019 (7)0.0013 (7)0.0042 (7)
C40.0181 (9)0.0089 (8)0.0248 (8)0.0004 (6)0.0016 (7)0.0006 (6)
C50.0141 (8)0.0126 (8)0.0202 (9)0.0019 (6)0.0009 (7)0.0057 (7)
N10.0095 (7)0.0138 (7)0.0129 (7)0.0008 (5)0.0001 (5)0.0009 (5)
N20.0093 (6)0.0133 (7)0.0152 (6)0.0012 (5)0.0004 (5)0.0020 (5)
Cl10.00792 (19)0.0140 (2)0.0183 (2)0.00061 (14)0.00025 (15)0.00070 (15)
Cl20.0135 (2)0.0135 (2)0.0173 (4)0.0000.0000.000
Cl30.0155 (2)0.0155 (2)0.0206 (4)0.0000.0000.000
Co10.00694 (16)0.00844 (16)0.00991 (17)0.00001 (10)0.00017 (11)0.00039 (11)
Geometric parameters (Å, º) top
C1—N11.4805 (18)C4—H4B0.975 (17)
C1—C21.502 (2)C5—N1i1.4784 (18)
C1—H1A0.965 (15)C5—H5A0.971 (16)
C1—H1B1.015 (15)C5—H5B0.949 (14)
C2—N21.4818 (18)N1—C5i1.4784 (18)
C2—H2A0.922 (15)N1—Co11.9697 (12)
C2—H2B0.995 (15)N1—H1C0.848 (15)
C3—N21.4839 (19)N2—Co11.9785 (12)
C3—C41.517 (2)N2—H2C0.807 (15)
C3—H3A0.973 (15)Cl1—Co12.2533 (4)
C3—H3B0.976 (15)Co1—N1i1.9697 (12)
C4—C51.509 (2)Co1—N2i1.9785 (12)
C4—H4A0.987 (17)Co1—Cl1i2.2533 (4)
N1—C1—C2107.42 (12)H5A—C5—H5B110.4 (12)
N1—C1—H1A107.9 (9)C5i—N1—C1111.32 (12)
C2—C1—H1A108.5 (9)C5i—N1—Co1118.79 (9)
N1—C1—H1B110.9 (8)C1—N1—Co1107.84 (9)
C2—C1—H1B109.0 (8)C5i—N1—H1C107.0 (10)
H1A—C1—H1B113.0 (12)C1—N1—H1C106.2 (10)
N2—C2—C1106.64 (12)Co1—N1—H1C104.9 (10)
N2—C2—H2A106.3 (9)C2—N2—C3111.14 (12)
C1—C2—H2A111.6 (9)C2—N2—Co1107.46 (9)
N2—C2—H2B110.6 (8)C3—N2—Co1119.61 (9)
C1—C2—H2B111.0 (9)C2—N2—H2C107.2 (11)
H2A—C2—H2B110.6 (12)C3—N2—H2C105.0 (11)
N2—C3—C4112.40 (12)Co1—N2—H2C105.7 (11)
N2—C3—H3A109.3 (9)N1—Co1—N1i180.00 (7)
C4—C3—H3A109.8 (9)N1—Co1—N2i93.77 (5)
N2—C3—H3B108.3 (9)N1i—Co1—N2i86.23 (5)
C4—C3—H3B110.0 (9)N1—Co1—N286.23 (5)
H3A—C3—H3B107.0 (12)N1i—Co1—N293.77 (5)
C5—C4—C3113.85 (13)N2i—Co1—N2180.00 (7)
C5—C4—H4A108.5 (9)N1—Co1—Cl188.43 (3)
C3—C4—H4A114.1 (9)N1i—Co1—Cl191.57 (3)
C5—C4—H4B107.7 (9)N2i—Co1—Cl188.40 (4)
C3—C4—H4B108.5 (9)N2—Co1—Cl191.60 (4)
H4A—C4—H4B103.5 (12)N1—Co1—Cl1i91.57 (3)
N1i—C5—C4111.16 (13)N1i—Co1—Cl1i88.43 (3)
N1i—C5—H5A106.7 (9)N2i—Co1—Cl1i91.60 (4)
C4—C5—H5A110.2 (9)N2—Co1—Cl1i88.40 (4)
N1i—C5—H5B106.5 (9)Cl1—Co1—Cl1i180.00 (2)
C4—C5—H5B111.7 (9)
N1—C1—C2—N254.18 (16)C5i—N1—Co1—Cl1127.11 (10)
N2—C3—C4—C566.02 (18)C1—N1—Co1—Cl1105.11 (9)
C3—C4—C5—N1i68.87 (17)C5i—N1—Co1—Cl1i52.89 (10)
C2—C1—N1—C5i171.91 (12)C1—N1—Co1—Cl1i74.89 (9)
C2—C1—N1—Co139.95 (14)C2—N2—Co1—N116.08 (9)
C1—C2—N2—C3174.35 (13)C3—N2—Co1—N1143.93 (11)
C1—C2—N2—Co141.75 (14)C2—N2—Co1—N1i163.92 (9)
C4—C3—N2—C2178.54 (13)C3—N2—Co1—N1i36.07 (11)
C4—C3—N2—Co152.40 (16)C2—N2—Co1—N2i7 (100)
C5i—N1—Co1—N1i41.13 (14)C3—N2—Co1—N2i135 (100)
C1—N1—Co1—N1i168.90 (12)C2—N2—Co1—Cl172.24 (9)
C5i—N1—Co1—N2i38.83 (11)C3—N2—Co1—Cl155.61 (10)
C1—N1—Co1—N2i166.60 (9)C2—N2—Co1—Cl1i107.76 (9)
C5i—N1—Co1—N2141.17 (11)C3—N2—Co1—Cl1i124.39 (10)
C1—N1—Co1—N213.40 (9)
Symmetry code: (i) x+1, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1C···Cl20.848 (15)2.693 (14)3.3251 (12)132.5 (12)
N2—H2C···Cl30.807 (15)2.757 (15)3.3638 (12)133.6 (13)
 

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