In the title complex, [Co(NH
2CH
2CH
2NH
2)
2(NO
2)
2](IO
4), the cations are situated on two sets of inversion centres and are linked by pairs of complementary N—H
O hydrogen bonds into columns arranged in an approximately hexagonal manner. The periodate anions can be envisaged as occupying triangular hollows above and below approximate hexagonal close-packed layers of
trans-bis(ethylenediamine-κ
2N,
N′)dinitrocobalt(III) cations.
Supporting information
CCDC reference: 245529
Key indicators
- Single-crystal X-ray study
- T = 180 K
- Mean (C-C) = 0.002 Å
- R factor = 0.015
- wR factor = 0.041
- Data-to-parameter ratio = 26.4
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT431_ALERT_2_B Short Inter HL..A Contact I1 .. O3 .. 3.11 Ang.
Alert level C
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co1 - N3 .. 6.66 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co2 - N5 .. 5.51 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Co2 - N6 .. 6.96 su
PLAT430_ALERT_2_C Short Inter D...A Contact O3 .. O3 .. 2.89 Ang.
PLAT431_ALERT_2_C Short Inter HL..A Contact I1 .. O1 .. 3.26 Ang.
PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 44.00 A 3
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
7 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: APEX2 (Bruker Nonius, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2000); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
trans-bis(ethylenediamine-
κ2N,
N')dinitrocobalt(III)
periodate
top
Crystal data top
[Co(C2H8N2)2(NO2)2](IO4) | Z = 2 |
Mr = 462.06 | F(000) = 452 |
Triclinic, P1 | Dx = 2.197 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.3556 (4) Å | Cell parameters from 6850 reflections |
b = 10.1773 (5) Å | θ = 3.1–33.2° |
c = 10.3602 (5) Å | µ = 3.49 mm−1 |
α = 79.123 (2)° | T = 180 K |
β = 74.383 (2)° | Block, yellow |
γ = 70.125 (2)° | 0.28 × 0.20 × 0.20 mm |
V = 698.39 (6) Å3 | |
Data collection top
Bruker Nonius X8 APEX-II CCD area-detector diffractometer | 4857 independent reflections |
Radiation source: fine-focus sealed tube | 4633 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.014 |
thin–slice ω and φ scans | θmax = 33.3°, θmin = 4.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | h = −10→10 |
Tmin = 0.429, Tmax = 0.498 | k = −15→15 |
7750 measured reflections | l = −15→14 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.015 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.041 | H-atom parameters constrained |
S = 1.11 | w = 1/[σ2(Fo2) + (0.0191P)2 + 0.1654P] where P = (Fo2 + 2Fc2)/3 |
4857 reflections | (Δ/σ)max = 0.002 |
184 parameters | Δρmax = 0.55 e Å−3 |
0 restraints | Δρmin = −0.78 e Å−3 |
Special details top
Experimental. All H atoms placed geometrically and refined using a riding model. |
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 | x | y | z | Uiso*/Ueq | |
Co1 | 0.0000 | 0.5000 | 0.5000 | 0.01212 (4) | |
N1 | −0.18028 (15) | 0.55178 (12) | 0.67214 (11) | 0.01626 (19) | |
H1C | −0.2302 | 0.4794 | 0.7147 | 0.020* | |
H1D | −0.1132 | 0.5690 | 0.7272 | 0.020* | |
N2 | −0.21867 (16) | 0.61717 (12) | 0.41803 (11) | 0.01695 (19) | |
H2C | −0.1892 | 0.6961 | 0.3704 | 0.020* | |
H2D | −0.2370 | 0.5684 | 0.3588 | 0.020* | |
C1 | −0.34488 (19) | 0.67993 (14) | 0.64610 (14) | 0.0200 (2) | |
H1A | −0.3005 | 0.7645 | 0.6283 | 0.024* | |
H1B | −0.4585 | 0.6913 | 0.7248 | 0.024* | |
C2 | −0.40350 (18) | 0.65938 (15) | 0.52372 (14) | 0.0210 (2) | |
H2A | −0.4697 | 0.5854 | 0.5468 | 0.025* | |
H2B | −0.4962 | 0.7478 | 0.4912 | 0.025* | |
N3 | 0.08672 (15) | 0.66230 (12) | 0.48960 (12) | 0.0175 (2) | |
O31 | 0.13963 (16) | 0.68218 (12) | 0.58610 (12) | 0.0270 (2) | |
O32 | 0.08403 (18) | 0.74833 (12) | 0.38688 (12) | 0.0296 (2) | |
Co2 | 0.0000 | 0.0000 | 0.0000 | 0.01378 (5) | |
N4 | 0.20032 (16) | −0.13540 (11) | 0.08996 (12) | 0.0175 (2) | |
H4C | 0.1442 | −0.1958 | 0.1526 | 0.021* | |
H4D | 0.3002 | −0.1876 | 0.0277 | 0.021* | |
N5 | 0.01491 (17) | 0.13782 (12) | 0.10228 (13) | 0.0194 (2) | |
H5A | 0.0845 | 0.1946 | 0.0464 | 0.023* | |
H5B | −0.1108 | 0.1936 | 0.1368 | 0.023* | |
C3 | 0.2834 (2) | −0.05981 (15) | 0.15784 (15) | 0.0214 (2) | |
H3A | 0.3888 | −0.0268 | 0.0925 | 0.026* | |
H3B | 0.3413 | −0.1230 | 0.2314 | 0.026* | |
C4 | 0.1154 (2) | 0.06346 (15) | 0.21380 (15) | 0.0232 (3) | |
H4A | 0.0217 | 0.0307 | 0.2906 | 0.028* | |
H4B | 0.1669 | 0.1268 | 0.2455 | 0.028* | |
N6 | −0.20998 (16) | −0.03784 (12) | 0.14519 (12) | 0.0195 (2) | |
O61 | −0.34406 (18) | 0.05964 (13) | 0.19964 (14) | 0.0362 (3) | |
O62 | −0.21024 (17) | −0.16080 (12) | 0.18326 (12) | 0.0282 (2) | |
I1 | 0.697895 (10) | 0.553556 (7) | 0.082435 (7) | 0.01332 (3) | |
O1 | 0.70196 (15) | 0.40058 (11) | 0.02204 (12) | 0.0257 (2) | |
O2 | 0.49868 (15) | 0.59377 (12) | 0.22472 (11) | 0.0239 (2) | |
O3 | 0.91623 (15) | 0.51966 (13) | 0.14096 (11) | 0.0257 (2) | |
O4 | 0.67200 (15) | 0.70025 (11) | −0.04195 (10) | 0.02182 (19) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co1 | 0.01199 (9) | 0.01423 (10) | 0.01017 (10) | −0.00494 (8) | −0.00134 (7) | −0.00126 (8) |
N1 | 0.0159 (4) | 0.0204 (5) | 0.0122 (4) | −0.0063 (4) | −0.0013 (4) | −0.0026 (4) |
N2 | 0.0169 (4) | 0.0194 (5) | 0.0144 (5) | −0.0054 (4) | −0.0043 (4) | −0.0005 (4) |
C1 | 0.0172 (5) | 0.0201 (6) | 0.0204 (6) | −0.0030 (4) | −0.0013 (4) | −0.0065 (5) |
C2 | 0.0143 (5) | 0.0259 (6) | 0.0212 (6) | −0.0036 (5) | −0.0036 (4) | −0.0038 (5) |
N3 | 0.0148 (4) | 0.0176 (5) | 0.0193 (5) | −0.0058 (4) | 0.0000 (4) | −0.0036 (4) |
O31 | 0.0297 (5) | 0.0293 (5) | 0.0292 (6) | −0.0143 (4) | −0.0084 (4) | −0.0075 (4) |
O32 | 0.0386 (6) | 0.0246 (5) | 0.0262 (6) | −0.0173 (5) | −0.0044 (5) | 0.0058 (4) |
Co2 | 0.01359 (9) | 0.00910 (9) | 0.01794 (11) | −0.00302 (7) | −0.00368 (8) | −0.00034 (8) |
N4 | 0.0181 (4) | 0.0121 (4) | 0.0217 (5) | −0.0028 (4) | −0.0068 (4) | 0.0000 (4) |
N5 | 0.0213 (5) | 0.0124 (5) | 0.0246 (6) | −0.0046 (4) | −0.0055 (4) | −0.0023 (4) |
C3 | 0.0201 (5) | 0.0198 (6) | 0.0268 (7) | −0.0069 (5) | −0.0094 (5) | −0.0007 (5) |
C4 | 0.0287 (6) | 0.0203 (6) | 0.0231 (7) | −0.0074 (5) | −0.0082 (5) | −0.0044 (5) |
N6 | 0.0174 (5) | 0.0196 (5) | 0.0215 (5) | −0.0065 (4) | −0.0052 (4) | 0.0004 (4) |
O61 | 0.0257 (5) | 0.0301 (6) | 0.0416 (7) | −0.0046 (4) | 0.0091 (5) | −0.0086 (5) |
O62 | 0.0343 (5) | 0.0227 (5) | 0.0290 (6) | −0.0154 (4) | −0.0074 (4) | 0.0069 (4) |
I1 | 0.01363 (4) | 0.01237 (4) | 0.01385 (4) | −0.00358 (3) | −0.00371 (3) | −0.00094 (3) |
O1 | 0.0249 (5) | 0.0150 (4) | 0.0395 (6) | −0.0041 (4) | −0.0087 (4) | −0.0100 (4) |
O2 | 0.0202 (4) | 0.0266 (5) | 0.0204 (5) | −0.0067 (4) | 0.0035 (4) | −0.0044 (4) |
O3 | 0.0185 (4) | 0.0389 (6) | 0.0201 (5) | −0.0039 (4) | −0.0092 (4) | −0.0061 (4) |
O4 | 0.0276 (5) | 0.0182 (4) | 0.0196 (5) | −0.0083 (4) | −0.0084 (4) | 0.0052 (4) |
Geometric parameters (Å, º) top
Co1—N3 | 1.9388 (11) | Co2—N4 | 1.9527 (11) |
Co1—N3i | 1.9388 (11) | Co2—N4ii | 1.9527 (11) |
Co1—N2 | 1.9441 (11) | Co2—N5 | 1.9572 (11) |
Co1—N2i | 1.9441 (11) | Co2—N5ii | 1.9572 (11) |
Co1—N1 | 1.9552 (10) | N4—C3 | 1.4885 (18) |
Co1—N1i | 1.9552 (11) | N4—H4C | 0.92 |
N1—C1 | 1.4863 (17) | N4—H4D | 0.92 |
N1—H1C | 0.92 | N5—C4 | 1.4845 (18) |
N1—H1D | 0.92 | N5—H5A | 0.92 |
N2—C2 | 1.4869 (17) | N5—H5B | 0.92 |
N2—H2C | 0.92 | C3—C4 | 1.507 (2) |
N2—H2D | 0.92 | C3—H3A | 0.99 |
C1—C2 | 1.514 (2) | C3—H3B | 0.99 |
C1—H1A | 0.99 | C4—H4A | 0.99 |
C1—H1B | 0.99 | C4—H4B | 0.99 |
C2—H2A | 0.99 | N6—O61 | 1.2335 (16) |
C2—H2B | 0.99 | N6—O62 | 1.2395 (15) |
N3—O31 | 1.2375 (15) | I1—O3 | 1.7705 (10) |
N3—O32 | 1.2440 (15) | I1—O4 | 1.7716 (10) |
Co2—N6ii | 1.9317 (11) | I1—O1 | 1.7726 (10) |
Co2—N6 | 1.9317 (11) | I1—O2 | 1.7734 (10) |
| | | |
N3—Co1—N3i | 180.0 | N6ii—Co2—N4ii | 90.95 (5) |
N3—Co1—N2 | 89.96 (5) | N6—Co2—N4ii | 89.05 (5) |
N3i—Co1—N2 | 90.04 (5) | N4—Co2—N4ii | 180.0 |
N3—Co1—N2i | 90.04 (5) | N6ii—Co2—N5 | 90.88 (5) |
N3i—Co1—N2i | 89.96 (5) | N6—Co2—N5 | 89.12 (5) |
N2—Co1—N2i | 180.0 | N4—Co2—N5 | 85.70 (5) |
N3—Co1—N1 | 88.61 (5) | N4ii—Co2—N5 | 94.30 (5) |
N3i—Co1—N1 | 91.39 (5) | N6ii—Co2—N5ii | 89.12 (5) |
N2—Co1—N1 | 85.94 (5) | N6—Co2—N5ii | 90.88 (5) |
N2i—Co1—N1 | 94.06 (5) | N4—Co2—N5ii | 94.30 (5) |
N3—Co1—N1i | 91.39 (5) | N4ii—Co2—N5ii | 85.70 (5) |
N3i—Co1—N1i | 88.61 (5) | N5—Co2—N5ii | 180.0 |
N2—Co1—N1i | 94.06 (5) | C3—N4—Co2 | 109.70 (8) |
N2i—Co1—N1i | 85.95 (5) | C3—N4—H4C | 109.7 |
N1—Co1—N1i | 180.0 | Co2—N4—H4C | 109.7 |
C1—N1—Co1 | 108.75 (8) | C3—N4—H4D | 109.7 |
C1—N1—H1C | 109.9 | Co2—N4—H4D | 109.7 |
Co1—N1—H1C | 109.9 | H4C—N4—H4D | 108.2 |
C1—N1—H1D | 109.9 | C4—N5—Co2 | 109.45 (8) |
Co1—N1—H1D | 109.9 | C4—N5—H5A | 109.8 |
H1C—N1—H1D | 108.3 | Co2—N5—H5A | 109.8 |
C2—N2—Co1 | 110.18 (8) | C4—N5—H5B | 109.8 |
C2—N2—H2C | 109.6 | Co2—N5—H5B | 109.8 |
Co1—N2—H2C | 109.6 | H5A—N5—H5B | 108.2 |
C2—N2—H2D | 109.6 | N4—C3—C4 | 107.30 (11) |
Co1—N2—H2D | 109.6 | N4—C3—H3A | 110.3 |
H2C—N2—H2D | 108.1 | C4—C3—H3A | 110.3 |
N1—C1—C2 | 106.24 (11) | N4—C3—H3B | 110.3 |
N1—C1—H1A | 110.5 | C4—C3—H3B | 110.3 |
C2—C1—H1A | 110.5 | H3A—C3—H3B | 108.5 |
N1—C1—H1B | 110.5 | N5—C4—C3 | 106.58 (12) |
C2—C1—H1B | 110.5 | N5—C4—H4A | 110.4 |
H1A—C1—H1B | 108.7 | C3—C4—H4A | 110.4 |
N2—C2—C1 | 107.24 (10) | N5—C4—H4B | 110.4 |
N2—C2—H2A | 110.3 | C3—C4—H4B | 110.4 |
C1—C2—H2A | 110.3 | H4A—C4—H4B | 108.6 |
N2—C2—H2B | 110.3 | O61—N6—O62 | 119.92 (12) |
C1—C2—H2B | 110.3 | O61—N6—Co2 | 120.37 (10) |
H2A—C2—H2B | 108.5 | O62—N6—Co2 | 119.71 (9) |
O31—N3—O32 | 120.11 (12) | O3—I1—O4 | 110.50 (5) |
O31—N3—Co1 | 120.15 (9) | O3—I1—O1 | 109.56 (5) |
O32—N3—Co1 | 119.71 (9) | O4—I1—O1 | 112.14 (5) |
N6ii—Co2—N6 | 180.00 (5) | O3—I1—O2 | 105.83 (5) |
N6ii—Co2—N4 | 89.05 (5) | O4—I1—O2 | 109.16 (5) |
N6—Co2—N4 | 90.95 (5) | O1—I1—O2 | 109.44 (5) |
| | | |
N3—Co1—N1—C1 | 71.41 (9) | N6ii—Co2—N4—C3 | 78.75 (9) |
N3i—Co1—N1—C1 | −108.59 (9) | N6—Co2—N4—C3 | −101.25 (9) |
N2—Co1—N1—C1 | −18.65 (9) | N5—Co2—N4—C3 | −12.21 (9) |
N2i—Co1—N1—C1 | 161.35 (9) | N5ii—Co2—N4—C3 | 167.79 (9) |
N3—Co1—N2—C2 | −98.21 (9) | N6ii—Co2—N5—C4 | −104.86 (9) |
N3i—Co1—N2—C2 | 81.79 (9) | N6—Co2—N5—C4 | 75.14 (9) |
N1—Co1—N2—C2 | −9.60 (9) | N4—Co2—N5—C4 | −15.88 (9) |
N1i—Co1—N2—C2 | 170.40 (9) | N4ii—Co2—N5—C4 | 164.12 (9) |
Co1—N1—C1—C2 | 42.03 (12) | Co2—N4—C3—C4 | 37.20 (13) |
Co1—N2—C2—C1 | 35.17 (13) | Co2—N5—C4—C3 | 39.90 (13) |
N1—C1—C2—N2 | −49.95 (14) | N4—C3—C4—N5 | −49.88 (14) |
N2—Co1—N3—O31 | 136.81 (10) | N4—Co2—N6—O61 | 129.13 (12) |
N2i—Co1—N3—O31 | −43.19 (10) | N4ii—Co2—N6—O61 | −50.87 (12) |
N1—Co1—N3—O31 | 50.87 (10) | N5—Co2—N6—O61 | 43.45 (12) |
N1i—Co1—N3—O31 | −129.13 (10) | N5ii—Co2—N6—O61 | −136.55 (12) |
N2—Co1—N3—O32 | −41.32 (10) | N4—Co2—N6—O62 | −51.22 (11) |
N2i—Co1—N3—O32 | 138.68 (10) | N4ii—Co2—N6—O62 | 128.78 (11) |
N1—Co1—N3—O32 | −127.26 (10) | N5—Co2—N6—O62 | −136.91 (11) |
N1i—Co1—N3—O32 | 52.74 (10) | N5ii—Co2—N6—O62 | 43.09 (11) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1C···O2i | 0.92 | 2.24 | 3.0390 (15) | 145 |
N1—H1D···O3iii | 0.92 | 2.12 | 2.9297 (15) | 146 |
N5—H5A···O4iv | 0.92 | 2.37 | 3.1347 (15) | 141 |
N4—H4D···O1v | 0.92 | 2.33 | 2.9258 (15) | 122 |
N2—H2D···O2vi | 0.92 | 2.60 | 3.3389 (16) | 138 |
N2—H2C···O62vii | 0.92 | 2.20 | 2.9943 (16) | 144 |
N5—H5B···O1vi | 0.92 | 2.39 | 3.0244 (16) | 126 |
N4—H4C···O32viii | 0.92 | 2.34 | 3.0809 (17) | 137 |
N4—H4D···O4viii | 0.92 | 2.54 | 3.3267 (15) | 144 |
Symmetry codes: (i) −x, −y+1, −z+1; (iii) −x+1, −y+1, −z+1; (iv) −x+1, −y+1, −z; (v) −x+1, −y, −z; (vi) x−1, y, z; (vii) x, y+1, z; (viii) x, y−1, z. |