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The crystal structure of the title compound, [Co(NCS)2(C4H12N2)2]ClO4, has been reported previously by Eminger, Fallab, Zehnder & Dobler [Helv. Chim. Acta (1992), 75, 1245–1250], with an R value of 0.074. However, no coordinates are available. We present here a redetermination of this structure using new intensity data. The CoIII atom, lying on an inversion centre, is six-coordinate in an octahedral geometry. The perchlorate anion, located on a twofold axis, is disordered over two orientations.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806008750/ci2007sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806008750/ci2007Isup2.hkl
Contains datablock I

CCDC reference: 605012

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](N-C) = 0.006 Å
  • Disorder in main residue
  • R factor = 0.052
  • wR factor = 0.138
  • Data-to-parameter ratio = 14.7

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT301_ALERT_3_B Main Residue Disorder ......................... 34.00 Perc. PLAT432_ALERT_2_B Short Inter X...Y Contact C3 .. O2' .. 2.87 Ang.
Alert level C PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C1 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C1' PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N2' PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 44.00 Perc. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 8 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 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Bis(N,N-dimethylethane-1,2-diamine)dithiocyanatocobalt(III) perchlorate top
Crystal data top
[Co(NCS)2(C4H12N2)2]ClO4F(000) = 936
Mr = 450.85Dx = 1.562 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 1131 reflections
a = 14.075 (3) Åθ = 2.3–20.4°
b = 11.481 (3) ŵ = 1.28 mm1
c = 12.366 (3) ÅT = 298 K
β = 106.380 (3)°Block, brown
V = 1917.2 (8) Å30.11 × 0.11 × 0.07 mm
Z = 4
Data collection top
Bruker SMART APEX area-detector
diffractometer
2199 independent reflections
Radiation source: fine-focus sealed tube1505 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
φ and ω scansθmax = 27.5°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1818
Tmin = 0.872, Tmax = 0.916k = 1414
8063 measured reflectionsl = 1615
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)] = 0.052Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.138H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0561P)2 + 3.9721P]
where P = (Fo2 + 2Fc2)/3
2199 reflections(Δ/σ)max = 0.001
150 parametersΔρmax = 0.55 e Å3
37 restraintsΔρmin = 0.36 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*/UeqOcc. (<1)
Co10.25000.25000.00000.0282 (2)
Cl10.00000.30076 (18)0.25000.0585 (5)
S10.38506 (9)0.24371 (10)0.38787 (9)0.0522 (3)
O10.0560 (6)0.3822 (7)0.2081 (7)0.125 (3)0.695 (7)
O20.0504 (7)0.2615 (8)0.1463 (6)0.141 (3)0.695 (7)
O1'0.1002 (8)0.3220 (17)0.2590 (16)0.125 (3)0.305 (7)
O2'0.0033 (15)0.1953 (11)0.1946 (15)0.141 (3)0.305 (7)
N10.3706 (2)0.1736 (3)0.0102 (3)0.0425 (8)
H1A0.38030.18910.07770.051*
H1B0.42270.20180.04360.051*
N30.3061 (3)0.2630 (3)0.1569 (3)0.0420 (8)
C10.3641 (4)0.0471 (4)0.0037 (6)0.0777 (18)0.637 (15)
H1C0.34530.01010.06980.093*0.637 (15)
H1D0.42840.01710.04540.093*0.637 (15)
C20.2912 (6)0.0182 (7)0.0640 (11)0.055 (3)0.637 (15)
H2A0.27540.06410.05480.066*0.637 (15)
H2B0.31970.03320.14380.066*0.637 (15)
N20.2006 (2)0.0859 (3)0.0228 (3)0.0399 (8)0.637 (15)
C30.1417 (8)0.0835 (8)0.1063 (8)0.057 (3)0.637 (15)
H3A0.12990.00420.12340.085*0.637 (15)
H3B0.07960.12220.07500.085*0.637 (15)
H3C0.17780.12260.17400.085*0.637 (15)
C40.1330 (8)0.0314 (10)0.0789 (7)0.056 (3)0.637 (15)
H4A0.11420.04470.06010.084*0.637 (15)
H4B0.16620.02470.13660.084*0.637 (15)
H4C0.07500.07880.10580.084*0.637 (15)
C1'0.3641 (4)0.0471 (4)0.0037 (6)0.0777 (18)0.363 (15)
H1'10.39710.00860.04550.093*0.363 (15)
H1'20.39960.02680.08070.093*0.363 (15)
C2'0.2702 (10)0.0052 (12)0.019 (2)0.058 (5)0.363 (15)
H2'10.27190.07050.01640.069*0.363 (15)
H2'20.24380.00540.09970.069*0.363 (15)
N2'0.2006 (2)0.0859 (3)0.0228 (3)0.0399 (8)0.363 (15)
C3'0.210 (2)0.0507 (14)0.1413 (9)0.072 (7)0.363 (15)
H3'A0.19120.02950.14300.108*0.363 (15)
H3'B0.16790.09860.17150.108*0.363 (15)
H3'C0.27770.06010.18580.108*0.363 (15)
C4'0.0988 (9)0.0579 (17)0.0466 (19)0.069 (6)0.363 (15)
H4'A0.08630.02370.04030.104*0.363 (15)
H4'B0.09220.07680.12400.104*0.363 (15)
H4'C0.05190.10240.02040.104*0.363 (15)
C50.3403 (3)0.2553 (3)0.2527 (4)0.0391 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0290 (4)0.0288 (4)0.0277 (4)0.0022 (3)0.0096 (3)0.0010 (3)
Cl10.0609 (10)0.0812 (12)0.0376 (8)0.0000.0206 (8)0.000
S10.0611 (7)0.0521 (7)0.0355 (6)0.0039 (6)0.0008 (5)0.0037 (5)
O10.149 (5)0.133 (6)0.117 (5)0.028 (4)0.078 (4)0.022 (4)
O20.156 (6)0.153 (6)0.091 (5)0.003 (5)0.004 (4)0.044 (4)
O1'0.149 (5)0.133 (6)0.117 (5)0.028 (4)0.078 (4)0.022 (4)
O2'0.156 (6)0.153 (6)0.091 (5)0.003 (5)0.004 (4)0.044 (4)
N10.0377 (18)0.043 (2)0.049 (2)0.0010 (15)0.0150 (15)0.0025 (16)
N30.0463 (19)0.048 (2)0.0299 (17)0.0052 (15)0.0073 (14)0.0034 (15)
C10.075 (4)0.038 (3)0.139 (6)0.012 (3)0.062 (4)0.002 (3)
C20.057 (5)0.032 (4)0.073 (7)0.006 (3)0.013 (5)0.006 (4)
N20.0442 (19)0.0323 (18)0.043 (2)0.0077 (15)0.0128 (15)0.0006 (15)
C30.064 (6)0.050 (5)0.068 (6)0.011 (4)0.036 (5)0.009 (4)
C40.062 (6)0.045 (5)0.055 (5)0.015 (5)0.008 (4)0.008 (4)
C1'0.075 (4)0.038 (3)0.139 (6)0.012 (3)0.062 (4)0.002 (3)
C2'0.047 (8)0.036 (7)0.090 (15)0.004 (6)0.019 (9)0.004 (8)
N2'0.0442 (19)0.0323 (18)0.043 (2)0.0077 (15)0.0128 (15)0.0006 (15)
C3'0.122 (18)0.040 (8)0.056 (9)0.024 (10)0.029 (10)0.010 (6)
C4'0.053 (9)0.040 (10)0.107 (17)0.016 (8)0.011 (9)0.000 (9)
C50.044 (2)0.0317 (19)0.041 (2)0.0029 (17)0.0105 (18)0.0037 (18)
Geometric parameters (Å, º) top
Co1—N11.946 (3)C1—H1C0.97
Co1—N22.055 (3)C1—H1D0.97
Co1—N3i1.883 (4)C2—N21.457 (8)
Co1—N31.883 (4)C2—H2A0.97
Co1—N1i1.946 (3)C2—H2B0.97
Co1—N2'i2.055 (3)N2—C41.485 (6)
Co1—N2i2.055 (3)N2—C31.495 (6)
Cl1—O21.355 (6)C3—H3A0.96
Cl1—O2ii1.355 (6)C3—H3B0.96
Cl1—O2'1.386 (8)C3—H3C0.96
Cl1—O2'ii1.386 (8)C4—H4A0.96
Cl1—O1'ii1.405 (8)C4—H4B0.96
Cl1—O1'1.405 (8)C4—H4C0.96
Cl1—O1ii1.412 (5)C2'—H2'10.97
Cl1—O11.412 (5)C2'—H2'20.97
S1—C51.616 (4)C3'—H3'A0.96
O2'—O2'ii1.35 (4)C3'—H3'B0.96
N1—C11.469 (6)C3'—H3'C0.96
N1—H1A0.90C4'—H4'A0.96
N1—H1B0.90C4'—H4'B0.96
N3—C51.150 (6)C4'—H4'C0.96
C1—C21.466 (10)
N1—Co1—N1i180O2'—Cl1—O1ii144.7 (9)
N2—Co1—N2i180O2'ii—Cl1—O1ii109.9 (10)
N3i—Co1—N3180O1'—Cl1—O1ii120.5 (9)
N1—Co1—N286.03 (13)O2—Cl1—O194.0 (5)
N3—Co1—N189.00 (14)O2ii—Cl1—O1111.7 (5)
N3—Co1—N289.46 (13)O2'—Cl1—O1109.9 (10)
N1i—Co1—N2i86.03 (13)O2'ii—Cl1—O1144.7 (9)
N3i—Co1—N191.00 (14)O1'ii—Cl1—O1120.5 (9)
N3i—Co1—N1i89.00 (14)O1ii—Cl1—O197.1 (8)
N3—Co1—N1i91.00 (14)O2'ii—O2'—Cl160.9 (8)
N3i—Co1—N290.54 (13)C1—N1—Co1110.7 (3)
N1i—Co1—N293.97 (13)C1—N1—H1A109.5
N3i—Co1—N2'i89.46 (13)Co1—N1—H1A109.5
N3—Co1—N2'i90.54 (13)C1—N1—H1B109.5
N1—Co1—N2'i93.97 (13)Co1—N1—H1B109.5
N1i—Co1—N2'i86.03 (13)H1A—N1—H1B108.1
N2—Co1—N2'i180.00 (19)C5—N3—Co1171.1 (3)
N3i—Co1—N2i89.46 (13)C2—C1—N1111.0 (5)
N3—Co1—N2i90.54 (13)C2—C1—H1C109.4
N1—Co1—N2i93.97 (13)N1—C1—H1C109.4
N2'i—Co1—N2i0.00 (19)C2—C1—H1D109.4
O2—Cl1—O2ii141.2 (8)N1—C1—H1D109.4
O2—Cl1—O2'46.1 (7)H1C—C1—H1D108.0
O2ii—Cl1—O2'96.5 (10)N2—C2—C1111.8 (7)
O2—Cl1—O2'ii96.5 (10)N2—C2—H2A109.3
O2ii—Cl1—O2'ii46.1 (7)C1—C2—H2A109.3
O2'—Cl1—O2'ii58.2 (17)N2—C2—H2B109.3
O2—Cl1—O1'ii74.8 (8)C1—C2—H2B109.3
O2ii—Cl1—O1'ii112.2 (9)H2A—C2—H2B107.9
O2'—Cl1—O1'ii102.7 (12)C2—N2—C4111.1 (6)
O2'ii—Cl1—O1'ii94.8 (10)C2—N2—C3110.5 (5)
O2—Cl1—O1'112.2 (9)C4—N2—C3103.3 (6)
O2ii—Cl1—O1'74.8 (8)C2—N2—Co1103.9 (4)
O2'—Cl1—O1'94.8 (10)C4—N2—Co1115.5 (5)
O2'ii—Cl1—O1'102.7 (12)C3—N2—Co1112.7 (4)
O1'ii—Cl1—O1'160.0 (16)H2'1—C2'—H2'2107.8
O2—Cl1—O1ii111.7 (5)N3—C5—S1178.3 (4)
O2ii—Cl1—O1ii94.0 (5)
Symmetry codes: (i) x+1/2, y+1/2, z; (ii) x, y, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1B···S1iii0.902.643.439 (3)148
N1—H1A···O1i0.902.343.217 (18)165
N1—H1A···O1i0.902.212.982 (8)143
Symmetry codes: (i) x+1/2, y+1/2, z; (iii) x+1, y, z+1/2.
 

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