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The hydro­thermal reaction of ethyl­enedi­amine with CoCl2·6H2O yielded tris­(ethyl­enedi­amine-κ2N,N′)­cobalt(III) chloride diiodide monohydrate, [Co(C2H8N2)3](Cl)(I)2·H2O, which consists of [Co(en)3]3+ cations, Cl and I anions, and solvent water mol­ecules. The Cl anions bridge the [Co(en)3]3+ complexes to form two-dimensional honeycomb-like layers through N—H...Cl hydrogen bonds, which stack along the c direction to form channels hosting I ions and water mol­ecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804030272/rz6010sup1.cif
Contains datablocks 182, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804030272/rz6010Isup2.hkl
Contains datablock I

CCDC reference: 262250

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.053
  • wR factor = 0.097
  • Data-to-parameter ratio = 19.1

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT230_ALERT_2_B Hirshfeld Test Diff for N11 - C11 .. 14.64 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Co2 - N21 .. 17.42 su PLAT415_ALERT_2_B Short Inter D-H..H-X H1 .. H21D .. 1.94 Ang. PLAT420_ALERT_2_B D-H Without Acceptor O1W - H1 ... ? PLAT601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 177.00 A   3
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.288 0.404 Tmin and Tmax expected: 0.209 0.404 RR = 1.379 Please check that your absorption correction is appropriate. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.35 PLAT213_ALERT_2_C Atom Cl1 has ADP max/min Ratio ............. 3.90 prolat PLAT751_ALERT_4_C Bond Calc 0.00000, Rep 0.0000(16) ...... Senseless su CL1 -CL1 1.555 1.555 PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C6 H24 Co N6 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C6 H24 Co N6 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 H2 O PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 I PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 5 Cl
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 25.03 From the CIF: _reflns_number_total 1588 Count of symmetry unique reflns 1027 Completeness (_total/calc) 154.63% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 561 Fraction of Friedel pairs measured 0.546 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 5 ALERT level B = Potentially serious problem 11 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 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 2 ALERT type 3 Indicator that the structure quality may be low 8 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: CrystalClear (Rigaku, 2002); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL; molecular graphics: Please provide missing details; software used to prepare material for publication: SHELXTL.

tris(ethylenediamine-κ2N,N')cobalt(III) chloride diiodide monohydrate top
Crystal data top
[Co(C2H8N2)3](Cl)(I)2·H2ODx = 2.020 Mg m3
Mr = 546.51Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6322Cell parameters from 425 reflections
Hall symbol: P 6c 2cθ = 3.2–27.5°
a = 11.2374 (8) ŵ = 4.54 mm1
c = 24.648 (3) ÅT = 293 K
V = 2695.5 (4) Å3Prism, orange
Z = 60.40 × 0.30 × 0.20 mm
F(000) = 1572
Data collection top
Rigaku Mercury CCD area-detector
diffractometer
1588 independent reflections
Radiation source: rotating-anode generator1081 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.099
ω scansθmax = 25.0°, θmin = 3.2°
Absorption correction: multi-scan
(SPHERE in CrystalClear; Rigaku, 2002)
h = 1313
Tmin = 0.288, Tmax = 0.404k = 1313
16790 measured reflectionsl = 2929
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.053H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.097 w = 1/[σ2(Fo2) + (0.0013P)2]
where P = (Fo2 + 2Fc2)/3
S = 1.01(Δ/σ)max = 0.003
1588 reflectionsΔρmax = 1.72 e Å3
83 parametersΔρmin = 0.93 e Å3
7 restraintsAbsolute structure: Flack (1983), with 578 Friedel pairs
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.09 (14)
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
Co11.66670.33330.40998 (4)0.0263 (3)
Co21.33330.66670.25000.0213 (4)
I11.57471 (3)0.69829 (3)0.42180 (1)0.03430 (8)
Cl11.55319 (7)1.10638 (14)0.25000.0384 (5)
N111.7259 (3)0.4990 (3)0.36442 (12)0.0331 (12)
H11A1.72020.47670.32910.040*
H11B1.67110.53480.37050.040*
N121.5471 (3)0.3732 (3)0.45566 (12)0.0272 (11)
H12A1.55840.36030.49090.033*
H12B1.56740.46080.45100.033*
N211.4782 (3)0.8025 (3)0.29543 (11)0.0313 (12)
H21A1.48520.88510.29030.038*
H21B1.45780.77940.33060.038*
C111.8665 (3)0.5981 (3)0.37847 (14)0.0249 (14)
H11C1.89040.68880.36540.030*
H11D1.92930.57220.36260.030*
C121.4026 (4)0.2762 (4)0.43824 (13)0.0307 (14)
H12C1.37080.18600.45380.037*
H12D1.34220.30940.45030.037*
C211.6117 (4)0.8106 (4)0.28177 (14)0.0347 (14)
H21C1.61740.73520.29820.042*
H21D1.68850.89670.29430.042*
O1W1.8830 (2)1.1170 (2)0.25000.091 (2)
H11.842 (3)1.0216 (4)0.2491 (16)0.071 (16)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.0317 (4)0.0317 (4)0.0154 (5)0.01584 (18)0.0000.000
Co20.0283 (5)0.0283 (5)0.0072 (6)0.0142 (3)0.0000.000
I10.05131 (11)0.04222 (11)0.01606 (10)0.02839 (9)0.00053 (15)0.00084 (13)
Cl10.0749 (10)0.0123 (8)0.0071 (7)0.0062 (4)0.0071 (7)0.000
N110.0456 (17)0.0441 (16)0.0195 (18)0.0299 (12)0.0100 (15)0.0064 (15)
N120.0375 (16)0.0212 (14)0.0304 (18)0.0203 (11)0.0030 (15)0.0068 (14)
N210.0544 (18)0.0367 (16)0.0118 (16)0.0294 (12)0.0125 (14)0.0112 (14)
C110.0165 (19)0.014 (2)0.027 (2)0.0047 (15)0.0035 (17)0.0063 (16)
C120.037 (2)0.0243 (18)0.027 (2)0.0126 (14)0.0129 (18)0.0065 (16)
C210.0226 (18)0.048 (2)0.0231 (19)0.0104 (14)0.0104 (16)0.0064 (18)
O1W0.0689 (18)0.0689 (18)0.134 (5)0.035 (2)0.025 (3)0.025 (3)
Geometric parameters (Å, º) top
Co1—N12i1.968 (4)N12—C121.497 (4)
Co1—N12ii1.968 (4)N12—H12A0.9000
Co1—N121.968 (4)N12—H12B0.9000
Co1—N11ii1.983 (3)N21—C211.496 (6)
Co1—N11i1.983 (3)N21—H21A0.9000
Co1—N111.983 (3)N21—H21B0.9000
Co2—N21iii1.936 (3)C11—C12ii1.476 (5)
Co2—N21iv1.936 (3)C11—H11C0.9700
Co2—N21v1.936 (3)C11—H11D0.9700
Co2—N211.936 (3)C12—C11i1.476 (5)
Co2—N21vi1.936 (3)C12—H12C0.9700
Co2—N21vii1.936 (3)C12—H12D0.9700
Cl1—Cl10.0000 (16)C21—C21vii1.570 (7)
N11—C111.449 (4)C21—H21C0.9700
N11—H11A0.9000C21—H21D0.9700
N11—H11B0.9000O1W—H10.932 (5)
N12i—Co1—N12ii90.52 (14)C11—N11—H11B110.1
N12i—Co1—N1290.52 (14)Co1—N11—H11B110.1
N12ii—Co1—N1290.52 (14)H11A—N11—H11B108.4
N12i—Co1—N11ii85.39 (11)C12—N12—Co1106.6 (2)
N12ii—Co1—N11ii93.27 (14)C12—N12—H12A110.4
N12—Co1—N11ii174.44 (12)Co1—N12—H12A110.4
N12i—Co1—N11i93.27 (14)C12—N12—H12B110.4
N12ii—Co1—N11i174.44 (12)Co1—N12—H12B110.4
N12—Co1—N11i85.39 (11)H12A—N12—H12B108.6
N11ii—Co1—N11i91.08 (13)C21—N21—Co2109.9 (2)
N12i—Co1—N11174.44 (12)C21—N21—H21A109.7
N12ii—Co1—N1185.39 (11)Co2—N21—H21A109.7
N12—Co1—N1193.27 (14)C21—N21—H21B109.7
N11ii—Co1—N1191.08 (13)Co2—N21—H21B109.7
N11i—Co1—N1191.08 (13)H21A—N21—H21B108.2
N21iii—Co2—N21iv86.6 (2)N11—C11—C12ii106.0 (3)
N21iii—Co2—N21v89.90 (11)N11—C11—H11C110.5
N21iv—Co2—N21v93.9 (2)C12ii—C11—H11C110.5
N21iii—Co2—N2193.9 (2)N11—C11—H11D110.5
N21iv—Co2—N2189.90 (11)C12ii—C11—H11D110.5
N21v—Co2—N21174.8 (2)H11C—C11—H11D108.7
N21iii—Co2—N21vi174.8 (2)C11i—C12—N12107.5 (3)
N21iv—Co2—N21vi89.90 (11)C11i—C12—H12C110.2
N21v—Co2—N21vi86.6 (2)N12—C12—H12C110.2
N21—Co2—N21vi89.90 (11)C11i—C12—H12D110.2
N21iii—Co2—N21vii89.90 (11)N12—C12—H12D110.2
N21iv—Co2—N21vii174.8 (2)H12C—C12—H12D108.5
N21v—Co2—N21vii89.90 (11)N21—C21—C21vii104.7 (3)
N21—Co2—N21vii86.6 (2)N21—C21—H21C110.8
N21vi—Co2—N21vii93.9 (2)C21vii—C21—H21C110.8
C11—N11—Co1108.1 (3)N21—C21—H21D110.8
C11—N11—H11A110.1C21vii—C21—H21D110.8
Co1—N11—H11A110.1H21C—C21—H21D108.9
Symmetry codes: (i) y+2, xy1, z; (ii) x+y+3, x+2, z; (iii) x+y+2, y, z+1/2; (iv) y+2, xy, z; (v) y+2, x+2, z+1/2; (vi) x+y+2, x+2, z; (vii) x, xy, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N21—H21A···Cl10.902.423.278 (4)160
N11—H11A···Cl1vi0.902.613.305 (3)135
Symmetry code: (vi) x+y+2, x+2, z.
 

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