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In the title compound, [Co(C2H3O2)2(C16H32N4)]I3, (I), the Co atom is six-coordinated by four N atoms from the tetradentate cyclo­tetradeca­diene ligand and two O atoms from two acetate ligands. The CoN4O2 coordination is octahedral. There are two independent centrosymmetric cations, and the anion lies in a general position.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804012899/cv6312sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804012899/cv6312Isup2.hkl
Contains datablock I

CCDC reference: 245142

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • R factor = 0.028
  • wR factor = 0.071
  • Data-to-parameter ratio = 18.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT380_ALERT_4_C Incorrectly Oriented X(sp2)-Methyl Moiety ...... C20 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C20 H38 Co N4 O4
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 4 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 3 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990).

Diacetato(5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-1,8- diene)cobalt(III) triiodide top
Crystal data top
[Co(C2H3O2)2(C16H32N4)]I3F(000) = 1616
Mr = 838.17Dx = 1.938 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 14.807 (3) ÅCell parameters from 3657 reflections
b = 9.7061 (18) Åθ = 2.3–26.2°
c = 20.218 (4) ŵ = 3.85 mm1
β = 98.589 (3)°T = 293 K
V = 2873.2 (9) Å3Diamond, purple
Z = 40.34 × 0.17 × 0.07 mm
Data collection top
Simens SMART CCD area detector
diffractometer
5656 independent reflections
Radiation source: fine-focus sealed tube4693 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.018
Detector resolution: 8.33 pixels mm-1θmax = 26.2°, θmin = 2.0°
ω scansh = 1812
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
k = 911
Tmin = 0.351, Tmax = 0.767l = 2424
15682 measured reflections
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)] = 0.028Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.071H-atom parameters constrained
S = 1.03 w = 1/[σ2(Fo2) + (0.0344P)2 + 1.6532P]
where P = (Fo2 + 2Fc2)/3
5656 reflections(Δ/σ)max = 0.002
300 parametersΔρmax = 0.66 e Å3
0 restraintsΔρmin = 0.40 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
I10.72168 (2)0.29171 (3)0.313713 (15)0.07831 (10)
I20.743465 (15)0.55713 (3)0.248211 (11)0.05948 (9)
I30.770407 (19)0.81075 (3)0.177762 (12)0.07069 (10)
Co11.50000.50000.50000.03152 (12)
Co21.00000.00000.50000.02949 (12)
O11.37309 (13)0.4742 (2)0.50398 (11)0.0413 (5)
O21.00432 (14)0.1733 (2)0.45476 (10)0.0408 (5)
O31.34901 (15)0.2485 (2)0.51361 (13)0.0584 (6)
O40.9188 (2)0.3193 (2)0.50294 (13)0.0691 (8)
N11.48610 (16)0.4465 (3)0.40608 (12)0.0382 (5)
N21.47031 (16)0.6952 (2)0.48081 (12)0.0369 (5)
H21.52600.73580.48290.037*
N30.87527 (15)0.0314 (2)0.45848 (11)0.0343 (5)
N41.05578 (15)0.0811 (2)0.42595 (11)0.0347 (5)
H41.06960.16850.44020.035*
C11.4657 (3)0.4713 (4)0.28377 (16)0.0646 (10)
H1A1.52060.49180.26580.065*
H1B1.41470.51510.25700.065*
H1C1.45620.37340.28350.065*
C21.4743 (2)0.5238 (3)0.35432 (15)0.0443 (7)
C31.4711 (2)0.6775 (4)0.36055 (16)0.0528 (8)
H3A1.44330.71410.31770.053*
H3B1.53360.71070.36850.053*
C41.4210 (2)0.7397 (3)0.41426 (16)0.0458 (7)
C51.3210 (2)0.6970 (4)0.40225 (17)0.0548 (9)
H5A1.31680.59830.40050.055*
H5B1.29190.73500.36060.055*
H5C1.29120.73070.43810.055*
C61.4287 (3)0.8981 (4)0.4088 (2)0.0688 (11)
H6A1.39340.94110.43920.069*
H6B1.40610.92650.36390.069*
H6C1.49150.92500.42000.069*
C71.4977 (2)0.2962 (3)0.40019 (16)0.0472 (8)
H7A1.52070.27430.35900.047*
H7B1.43970.24970.39990.047*
C81.5646 (2)0.2509 (3)0.45942 (16)0.0458 (7)
H8A1.56860.15120.46110.046*
H8B1.62490.28790.45680.046*
C91.3227 (2)0.3687 (3)0.50999 (15)0.0424 (7)
C101.2248 (2)0.4032 (4)0.5133 (2)0.0593 (9)
H10A1.18750.32370.50120.059*
H10B1.20570.47710.48280.059*
H10C1.21870.43100.55800.059*
C110.7494 (2)0.0967 (4)0.37088 (17)0.0530 (8)
H11A0.73150.19070.36160.053*
H11B0.74250.04550.32980.053*
H11C0.71150.05690.40050.053*
C120.8475 (2)0.0923 (3)0.40330 (15)0.0408 (7)
C130.9133 (2)0.1714 (3)0.36710 (16)0.0460 (7)
H13A0.88140.19620.32330.046*
H13B0.92850.25660.39130.046*
C141.0020 (2)0.1017 (3)0.35733 (14)0.0402 (7)
C150.9844 (2)0.0316 (4)0.31841 (16)0.0551 (9)
H15A0.94820.09190.34150.055*
H15B0.95220.01210.27460.055*
H15C1.04150.07530.31450.055*
C161.0547 (3)0.2025 (4)0.31823 (17)0.0580 (9)
H16A1.11080.16050.31020.058*
H16B1.01810.22460.27630.058*
H16C1.06810.28520.34390.058*
C170.8093 (2)0.0227 (3)0.49979 (15)0.0437 (7)
H17A0.75400.03230.49340.044*
H17B0.79340.11710.48740.044*
C180.8541 (2)0.0158 (3)0.57140 (15)0.0430 (7)
H18A0.81770.06450.60000.043*
H18B0.86070.07930.58620.043*
C190.9650 (2)0.2893 (3)0.45977 (15)0.0410 (7)
C200.9807 (3)0.3935 (3)0.40775 (18)0.0555 (9)
H20A0.92310.42090.38300.055*
H20B1.01800.35360.37780.055*
H20C1.01100.47270.42920.055*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
I10.06814 (19)0.0837 (2)0.0838 (2)0.01460 (15)0.01380 (15)0.00436 (15)
I20.04590 (14)0.07755 (18)0.05422 (15)0.00504 (11)0.00491 (10)0.02104 (12)
I30.06798 (18)0.0887 (2)0.05275 (15)0.01068 (14)0.00023 (12)0.00215 (13)
Co10.0269 (3)0.0310 (3)0.0361 (3)0.0009 (2)0.0029 (2)0.0031 (2)
Co20.0293 (3)0.0252 (3)0.0343 (3)0.0003 (2)0.0058 (2)0.0029 (2)
O10.0286 (10)0.0385 (11)0.0563 (13)0.0010 (9)0.0044 (9)0.0039 (9)
O20.0455 (12)0.0291 (11)0.0493 (12)0.0020 (9)0.0118 (10)0.0039 (9)
O30.0431 (13)0.0424 (14)0.0906 (18)0.0052 (11)0.0131 (12)0.0081 (12)
O40.096 (2)0.0418 (14)0.0757 (17)0.0245 (13)0.0350 (16)0.0082 (12)
N10.0332 (13)0.0412 (14)0.0393 (13)0.0023 (11)0.0030 (10)0.0001 (11)
N20.0321 (13)0.0335 (13)0.0441 (13)0.0018 (10)0.0024 (10)0.0037 (10)
N30.0319 (12)0.0308 (12)0.0408 (13)0.0009 (10)0.0069 (10)0.0017 (10)
N40.0366 (13)0.0311 (12)0.0372 (12)0.0004 (10)0.0081 (10)0.0040 (10)
C10.071 (3)0.081 (3)0.0416 (19)0.015 (2)0.0074 (17)0.0035 (18)
C20.0331 (16)0.059 (2)0.0405 (16)0.0064 (14)0.0036 (13)0.0038 (15)
C30.053 (2)0.059 (2)0.0445 (17)0.0013 (16)0.0028 (15)0.0152 (16)
C40.0424 (17)0.0398 (17)0.0522 (18)0.0038 (14)0.0028 (14)0.0121 (14)
C50.0438 (19)0.057 (2)0.060 (2)0.0147 (16)0.0048 (16)0.0027 (17)
C60.082 (3)0.044 (2)0.076 (3)0.0057 (19)0.004 (2)0.0169 (19)
C70.053 (2)0.0408 (18)0.0479 (18)0.0008 (14)0.0065 (15)0.0062 (14)
C80.0472 (18)0.0341 (16)0.0568 (19)0.0071 (14)0.0100 (15)0.0033 (14)
C90.0341 (16)0.049 (2)0.0445 (17)0.0054 (14)0.0060 (13)0.0018 (14)
C100.0346 (17)0.061 (2)0.083 (3)0.0040 (16)0.0109 (17)0.0059 (19)
C110.0416 (18)0.065 (2)0.0495 (18)0.0068 (16)0.0013 (14)0.0000 (16)
C120.0389 (16)0.0404 (17)0.0423 (16)0.0069 (13)0.0034 (13)0.0031 (13)
C130.0497 (18)0.0457 (18)0.0411 (16)0.0061 (15)0.0021 (14)0.0083 (14)
C140.0461 (17)0.0413 (17)0.0338 (15)0.0019 (13)0.0084 (13)0.0050 (13)
C150.061 (2)0.060 (2)0.0426 (18)0.0035 (17)0.0029 (16)0.0035 (15)
C160.064 (2)0.063 (2)0.0493 (19)0.0022 (18)0.0163 (17)0.0177 (17)
C170.0312 (15)0.0450 (18)0.0548 (18)0.0004 (13)0.0063 (13)0.0093 (14)
C180.0379 (16)0.0466 (18)0.0473 (17)0.0007 (13)0.0151 (13)0.0036 (14)
C190.0451 (17)0.0309 (16)0.0455 (17)0.0006 (13)0.0016 (14)0.0031 (13)
C200.065 (2)0.0368 (18)0.064 (2)0.0012 (16)0.0063 (18)0.0110 (16)
Geometric parameters (Å, º) top
I1—I22.9364 (6)C5—H5C0.9600
I2—I32.9012 (6)C6—H6A0.9600
Co1—O1i1.9095 (19)C6—H6B0.9600
Co1—O11.9095 (19)C6—H6C0.9600
Co1—N11.950 (2)C7—C81.501 (4)
Co1—N1i1.950 (2)C7—H7A0.9700
Co1—N21.970 (2)C7—H7B0.9700
Co1—N2i1.970 (2)C8—N2i1.480 (4)
Co2—O2ii1.920 (2)C8—H8A0.9700
Co2—O21.920 (2)C8—H8B0.9700
Co2—N31.935 (2)C9—C101.499 (4)
Co2—N3ii1.935 (2)C10—H10A0.9600
Co2—N41.978 (2)C10—H10B0.9600
Co2—N4ii1.978 (2)C10—H10C0.9600
O1—C91.283 (4)C11—C121.502 (4)
O2—C191.279 (3)C11—H11A0.9600
O3—C91.229 (4)C11—H11B0.9600
O4—C191.221 (4)C11—H11C0.9600
N1—C21.278 (4)C12—C131.513 (4)
N1—C71.476 (4)C13—C141.517 (4)
N2—C8i1.480 (4)C13—H13A0.9700
N2—C41.496 (4)C13—H13B0.9700
N2—H20.9100C14—C151.516 (4)
N3—C121.276 (4)C14—C161.541 (4)
N3—C171.473 (4)C15—H15A0.9600
N4—C18ii1.472 (4)C15—H15B0.9600
N4—C141.506 (4)C15—H15C0.9600
N4—H40.9100C16—H16A0.9600
C1—C21.502 (5)C16—H16B0.9600
C1—H1A0.9600C16—H16C0.9600
C1—H1B0.9600C17—C181.501 (4)
C1—H1C0.9600C17—H17A0.9700
C2—C31.498 (5)C17—H17B0.9700
C3—C41.528 (5)C18—N4ii1.472 (4)
C3—H3A0.9700C18—H18A0.9700
C3—H3B0.9700C18—H18B0.9700
C4—C51.521 (4)C19—C201.502 (4)
C4—C61.547 (5)C20—H20A0.9600
C5—H5A0.9600C20—H20B0.9600
C5—H5B0.9600C20—H20C0.9600
I3—I2—I1176.599 (12)H6A—C6—H6B109.5
O1i—Co1—O1180C4—C6—H6C109.5
O1i—Co1—N187.43 (9)H6A—C6—H6C109.5
O1—Co1—N192.57 (9)H6B—C6—H6C109.5
O1i—Co1—N1i92.57 (9)N1—C7—C8107.2 (2)
O1—Co1—N1i87.43 (9)N1—C7—H7A110.3
N1—Co1—N1i180C8—C7—H7A110.3
O1i—Co1—N293.30 (9)N1—C7—H7B110.3
O1—Co1—N286.70 (9)C8—C7—H7B110.3
N1—Co1—N294.37 (10)H7A—C7—H7B108.5
N1i—Co1—N285.63 (10)N2i—C8—C7106.1 (2)
O1i—Co1—N2i86.70 (9)N2i—C8—H8A110.5
O1—Co1—N2i93.30 (9)C7—C8—H8A110.5
N1—Co1—N2i85.63 (10)N2i—C8—H8B110.5
N1i—Co1—N2i94.37 (10)C7—C8—H8B110.5
N2—Co1—N2i180H8A—C8—H8B108.7
O2ii—Co2—O2180O3—C9—O1125.4 (3)
O2ii—Co2—N388.36 (9)O3—C9—C10120.6 (3)
O2—Co2—N391.64 (9)O1—C9—C10113.9 (3)
O2ii—Co2—N3ii91.64 (9)C9—C10—H10A109.5
O2—Co2—N3ii88.36 (9)C9—C10—H10B109.5
N3—Co2—N3ii180H10A—C10—H10B109.5
O2ii—Co2—N493.41 (9)C9—C10—H10C109.5
O2—Co2—N486.59 (9)H10A—C10—H10C109.5
N3—Co2—N495.08 (9)H10B—C10—H10C109.5
N3ii—Co2—N484.92 (9)C12—C11—H11A109.5
O2ii—Co2—N4ii86.59 (9)C12—C11—H11B109.5
O2—Co2—N4ii93.41 (9)H11A—C11—H11B109.5
N3—Co2—N4ii84.92 (9)C12—C11—H11C109.5
N3ii—Co2—N4ii95.08 (9)H11A—C11—H11C109.5
N4—Co2—N4ii180H11B—C11—H11C109.5
C9—O1—Co1134.3 (2)N3—C12—C11124.0 (3)
C19—O2—Co2133.3 (2)N3—C12—C13120.8 (3)
C2—N1—C7121.2 (3)C11—C12—C13115.2 (3)
C2—N1—Co1128.5 (2)C12—C13—C14118.0 (3)
C7—N1—Co1110.19 (19)C12—C13—H13A107.8
C8i—N2—C4116.7 (2)C14—C13—H13A107.8
C8i—N2—Co1105.93 (18)C12—C13—H13B107.8
C4—N2—Co1121.29 (19)C14—C13—H13B107.8
C8i—N2—H2103.5H13A—C13—H13B107.1
C4—N2—H2103.5N4—C14—C15113.0 (2)
Co1—N2—H2103.5N4—C14—C13106.7 (2)
C12—N3—C17120.4 (2)C15—C14—C13111.3 (3)
C12—N3—Co2127.9 (2)N4—C14—C16108.6 (3)
C17—N3—Co2111.63 (18)C15—C14—C16109.7 (3)
C18ii—N4—C14116.3 (2)C13—C14—C16107.3 (3)
C18ii—N4—Co2106.27 (17)C14—C15—H15A109.5
C14—N4—Co2121.81 (18)C14—C15—H15B109.5
C18ii—N4—H4103.3H15A—C15—H15B109.5
C14—N4—H4103.3C14—C15—H15C109.5
Co2—N4—H4103.3H15A—C15—H15C109.5
C2—C1—H1A109.5H15B—C15—H15C109.5
C2—C1—H1B109.5C14—C16—H16A109.5
H1A—C1—H1B109.5C14—C16—H16B109.5
C2—C1—H1C109.5H16A—C16—H16B109.5
H1A—C1—H1C109.5C14—C16—H16C109.5
H1B—C1—H1C109.5H16A—C16—H16C109.5
N1—C2—C3121.2 (3)H16B—C16—H16C109.5
N1—C2—C1124.0 (3)N3—C17—C18107.2 (2)
C3—C2—C1114.7 (3)N3—C17—H17A110.3
C2—C3—C4118.5 (3)C18—C17—H17A110.3
C2—C3—H3A107.7N3—C17—H17B110.3
C4—C3—H3A107.7C18—C17—H17B110.3
C2—C3—H3B107.7H17A—C17—H17B108.5
C4—C3—H3B107.7N4ii—C18—C17106.5 (2)
H3A—C3—H3B107.1N4ii—C18—H18A110.4
N2—C4—C5113.4 (3)C17—C18—H18A110.4
N2—C4—C3107.6 (2)N4ii—C18—H18B110.4
C5—C4—C3110.1 (3)C17—C18—H18B110.4
N2—C4—C6108.6 (3)H18A—C18—H18B108.6
C5—C4—C6109.9 (3)O4—C19—O2125.2 (3)
C3—C4—C6107.0 (3)O4—C19—C20120.1 (3)
C4—C5—H5A109.5O2—C19—C20114.7 (3)
C4—C5—H5B109.5C19—C20—H20A109.5
H5A—C5—H5B109.5C19—C20—H20B109.5
C4—C5—H5C109.5H20A—C20—H20B109.5
H5A—C5—H5C109.5C19—C20—H20C109.5
H5B—C5—H5C109.5H20A—C20—H20C109.5
C4—C6—H6A109.5H20B—C20—H20C109.5
C4—C6—H6B109.5
Symmetry codes: (i) x+3, y+1, z+1; (ii) x+2, y, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O3i0.911.852.716 (3)159
N4—H4···O4ii0.911.852.719 (3)158
C5—H5A···O10.962.453.005 (4)117
C8—H8B···O1i0.972.442.883 (4)107
C15—H15A···O20.962.453.055 (4)121
C17—H17A···O3ii0.972.593.508 (4)159
C18—H18B···O2ii0.972.452.894 (4)107
C20—H20C···O4iii0.962.573.527 (4)174
Symmetry codes: (i) x+3, y+1, z+1; (ii) x+2, y, z+1; (iii) x+2, y+1, z+1.
 

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