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The crystal structures of the first-row transition-metal series of tris­(ethyl­enedi­amine-κ2N,N′)metal(II) di­acetate, [M(C2H8N2)3](CH3CO2)2, with M = Mn, Fe, Co, Ni, Cu, and Zn, are reported. The complexes are all isostructural, crystallizing in a centrosymmetric triclinic cell and possessing an asymmetric unit composed of one [M(en)3]2+ cation and two symmetrically independent acetate anions. In the unit cell, the two complex cations are inversion-generated enanti­omers, possessing the energetically favoured Δ(λλλ) and Λ(δδδ) configurations. The complex cations and acetate anions combine through a series of N—H...O hydrogen bonds to generate a three-dimensional network in the crystals. The other notable feature of the series is a significant Jahn–Teller distortion for the d9 Cu2+ complex.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229617006738/yp3135sup1.cif
Contains datablocks umd905_a, umd815, umd906_a, umd908, umd943_a, umd886

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617006738/yp3135umd905_asup2.hkl
Contains datablock umd905_a

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617006738/yp3135umd815sup3.hkl
Contains datablock umd815

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617006738/yp3135umd906_asup4.hkl
Contains datablock umd906_a

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617006738/yp3135umd908sup5.hkl
Contains datablock umd908

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617006738/yp3135umd943_asup6.hkl
Contains datablock umd943_a

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229617006738/yp3135umd886sup7.hkl
Contains datablock umd886

CCDC references: 1547938; 1547937; 1547936; 1547935; 1547934; 1547933

Computing details top

For all structures, data collection: APEX2 (Bruker, 2014); cell refinement: SAINT (Bruker, 2014); data reduction: SAINT (Bruker, 2014); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008). Molecular graphics: SHELXTL (Sheldrick, 2008) for umd905_a, umd815, umd908, umd943_a, umd886; OLEX2 (Dolomanov et al., 2009) for umd906_a. Software used to prepare material for publication: SHELXTL (Sheldrick, 2008) for umd905_a, umd815, umd908, umd943_a, umd886; OLEX2 (Dolomanov et al., 2009) for umd906_a.

Tris(ethylenediamine-κ2N,N')manganese(II) diacetate (umd905_a) top
Crystal data top
[Mn(C2H8N2)3](C2H3O2)2Z = 2
Mr = 353.34F(000) = 378
Triclinic, P1Dx = 1.298 Mg m3
a = 8.3860 (9) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.1422 (9) ÅCell parameters from 9895 reflections
c = 12.9405 (14) Åθ = 3.0–25.5°
α = 69.526 (4)°µ = 0.75 mm1
β = 87.160 (4)°T = 200 K
γ = 76.788 (4)°Block, colourless
V = 904.33 (16) Å30.28 × 0.20 × 0.18 mm
Data collection top
Bruker CMOS
diffractometer
3332 independent reflections
Radiation source: fine-focus sealed tube3047 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.030
φ and ω scansθmax = 25.5°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2014)
h = 1010
Tmin = 0.817, Tmax = 0.877k = 1111
25301 measured reflectionsl = 1515
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)] = 0.023H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.060 w = 1/[σ2(Fo2) + (0.0254P)2 + 0.3555P]
where P = (Fo2 + 2Fc2)/3
S = 1.05(Δ/σ)max = 0.001
3332 reflectionsΔρmax = 0.29 e Å3
229 parametersΔρmin = 0.18 e Å3
12 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.017 (2)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Mn10.56819 (2)0.64374 (2)0.712668 (16)0.02420 (9)
O10.73843 (14)0.04560 (14)0.55454 (10)0.0425 (3)
O20.69158 (18)0.26521 (16)0.59452 (14)0.0689 (5)
N10.53719 (16)0.69532 (15)0.87081 (10)0.0308 (3)
H1NB0.4532 (16)0.663 (2)0.9065 (13)0.037*
H1NA0.6238 (15)0.6452 (18)0.9131 (12)0.037*
N20.44821 (15)0.90987 (15)0.65172 (10)0.0296 (3)
H2NB0.3727 (16)0.930 (2)0.6015 (11)0.036*
H2NA0.5213 (17)0.9641 (18)0.6213 (13)0.036*
N30.62665 (14)0.61548 (15)0.54673 (10)0.0263 (3)
H3NB0.639 (2)0.5156 (12)0.5547 (13)0.032*
H3NA0.5457 (15)0.6685 (17)0.4992 (11)0.032*
N40.82619 (15)0.68812 (15)0.68501 (10)0.0299 (3)
H4NB0.8909 (18)0.6576 (19)0.7426 (10)0.036*
H4NA0.815 (2)0.7910 (11)0.6536 (13)0.036*
N50.62220 (18)0.37546 (16)0.80588 (11)0.0366 (3)
H5NB0.674 (2)0.322 (2)0.7663 (13)0.044*
H5NA0.6819 (19)0.352 (2)0.8645 (11)0.044*
N60.32040 (16)0.58508 (18)0.70418 (11)0.0375 (3)
H6NB0.2509 (19)0.621 (2)0.7469 (13)0.045*
H6NA0.279 (2)0.632 (2)0.6373 (9)0.045*
C10.5093 (2)0.86951 (19)0.84352 (13)0.0387 (4)
H1B0.61340.90430.82270.046*
H1A0.46800.89830.90850.046*
C20.3843 (2)0.95266 (19)0.74796 (13)0.0379 (4)
H2A0.27970.91890.76930.046*
H2B0.36311.07020.72910.046*
C30.77921 (17)0.66671 (18)0.50754 (12)0.0303 (3)
H3B0.75560.78470.47150.036*
H3A0.82730.61820.45240.036*
C40.90019 (17)0.61537 (19)0.60379 (12)0.0323 (3)
H4B0.92720.49710.63840.039*
H4A1.00270.65070.57750.039*
C50.4636 (2)0.3318 (2)0.83653 (13)0.0428 (4)
H5B0.41950.36690.89850.051*
H5A0.47870.21400.86100.051*
C60.3439 (2)0.4108 (2)0.73861 (13)0.0417 (4)
H6B0.38690.37450.67690.050*
H6A0.23760.38020.75900.050*
C70.9441 (2)0.0783 (2)0.65646 (17)0.0503 (5)
H7A0.96950.16550.67540.075*
H7B1.02830.04580.60850.075*
H7C0.94170.01330.72410.075*
C80.77878 (17)0.13513 (16)0.59685 (11)0.0275 (3)
O30.06899 (15)0.67463 (17)0.85093 (10)0.0515 (3)
O40.24077 (13)0.62274 (15)0.98985 (9)0.0437 (3)
C100.0381 (2)0.7387 (3)1.00606 (18)0.0649 (6)
H10A0.13400.79520.95610.097*
H10B0.00470.81311.03520.097*
H10C0.06580.64971.06730.097*
C90.10177 (18)0.67380 (19)0.94349 (12)0.0334 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.02426 (13)0.02828 (13)0.02108 (12)0.00336 (8)0.00323 (8)0.01091 (9)
O10.0480 (7)0.0409 (6)0.0435 (7)0.0104 (5)0.0117 (5)0.0189 (5)
O20.0623 (9)0.0453 (8)0.1023 (12)0.0180 (6)0.0411 (8)0.0425 (8)
N10.0340 (7)0.0347 (7)0.0222 (6)0.0018 (5)0.0055 (5)0.0110 (5)
N20.0299 (7)0.0320 (7)0.0251 (6)0.0027 (5)0.0068 (5)0.0093 (5)
N30.0252 (6)0.0314 (6)0.0244 (6)0.0039 (5)0.0040 (5)0.0130 (5)
N40.0265 (6)0.0339 (7)0.0311 (7)0.0040 (5)0.0090 (5)0.0138 (6)
N50.0491 (8)0.0323 (7)0.0268 (7)0.0036 (6)0.0106 (6)0.0105 (6)
N60.0319 (7)0.0522 (8)0.0298 (7)0.0128 (6)0.0041 (5)0.0131 (6)
C10.0530 (10)0.0378 (9)0.0287 (8)0.0067 (7)0.0059 (7)0.0172 (7)
C20.0438 (9)0.0321 (8)0.0347 (8)0.0035 (7)0.0037 (7)0.0147 (7)
C30.0276 (7)0.0386 (8)0.0263 (7)0.0050 (6)0.0013 (6)0.0150 (6)
C40.0219 (7)0.0389 (8)0.0363 (8)0.0014 (6)0.0025 (6)0.0163 (7)
C50.0677 (12)0.0402 (9)0.0258 (8)0.0257 (8)0.0006 (8)0.0092 (7)
C60.0491 (10)0.0574 (11)0.0319 (8)0.0289 (8)0.0031 (7)0.0211 (8)
C70.0377 (9)0.0411 (9)0.0676 (12)0.0101 (7)0.0207 (9)0.0096 (9)
C80.0272 (7)0.0262 (7)0.0266 (7)0.0073 (6)0.0026 (6)0.0048 (6)
O30.0437 (7)0.0796 (9)0.0331 (6)0.0129 (6)0.0099 (5)0.0213 (6)
O40.0318 (6)0.0631 (8)0.0322 (6)0.0055 (5)0.0088 (5)0.0136 (5)
C100.0455 (11)0.0860 (16)0.0622 (13)0.0029 (10)0.0068 (10)0.0328 (12)
C90.0316 (8)0.0384 (8)0.0269 (8)0.0088 (6)0.0037 (6)0.0061 (6)
Geometric parameters (Å, º) top
Mn1—N12.2459 (12)C1—C21.521 (2)
Mn1—N32.2680 (12)C1—H1B0.9900
Mn1—N52.2699 (13)C1—H1A0.9900
Mn1—N22.2740 (13)C2—H2A0.9900
Mn1—N62.2784 (13)C2—H2B0.9900
Mn1—N42.2797 (13)C3—C41.5164 (19)
O1—C81.2421 (17)C3—H3B0.9900
O2—C81.2368 (18)C3—H3A0.9900
N1—C11.470 (2)C4—H4B0.9900
N1—H1NB0.875 (9)C4—H4A0.9900
N1—H1NA0.866 (9)C5—C61.513 (2)
N2—C21.4731 (19)C5—H5B0.9900
N2—H2NB0.872 (9)C5—H5A0.9900
N2—H2NA0.869 (9)C6—H6B0.9900
N3—C31.4686 (19)C6—H6A0.9900
N3—H3NB0.863 (9)C7—C81.511 (2)
N3—H3NA0.869 (9)C7—H7A0.9800
N4—C41.4724 (19)C7—H7B0.9800
N4—H4NB0.868 (9)C7—H7C0.9800
N4—H4NA0.868 (9)O3—C91.2392 (19)
N5—C51.472 (2)O4—C91.2495 (18)
N5—H5NB0.866 (9)C10—C91.519 (2)
N5—H5NA0.865 (9)C10—H10A0.9800
N6—C61.464 (2)C10—H10B0.9800
N6—H6NB0.871 (9)C10—H10C0.9800
N6—H6NA0.871 (9)
N1—Mn1—N3171.45 (5)C2—C1—H1B109.9
N1—Mn1—N591.55 (5)N1—C1—H1A109.9
N3—Mn1—N593.58 (5)C2—C1—H1A109.9
N1—Mn1—N278.00 (5)H1B—C1—H1A108.3
N3—Mn1—N298.52 (4)N2—C2—C1109.23 (12)
N5—Mn1—N2162.89 (5)N2—C2—H2A109.8
N1—Mn1—N698.33 (5)C1—C2—H2A109.8
N3—Mn1—N689.45 (5)N2—C2—H2B109.8
N5—Mn1—N677.81 (5)C1—C2—H2B109.8
N2—Mn1—N690.21 (5)H2A—C2—H2B108.3
N1—Mn1—N494.92 (5)N3—C3—C4109.91 (12)
N3—Mn1—N477.37 (4)N3—C3—H3B109.7
N5—Mn1—N4101.35 (5)C4—C3—H3B109.7
N2—Mn1—N493.11 (5)N3—C3—H3A109.7
N6—Mn1—N4166.74 (5)C4—C3—H3A109.7
C1—N1—Mn1108.21 (9)H3B—C3—H3A108.2
C1—N1—H1NB108.8 (11)N4—C4—C3108.81 (11)
Mn1—N1—H1NB111.3 (11)N4—C4—H4B109.9
C1—N1—H1NA111.3 (11)C3—C4—H4B109.9
Mn1—N1—H1NA109.5 (11)N4—C4—H4A109.9
H1NB—N1—H1NA107.8 (16)C3—C4—H4A109.9
C2—N2—Mn1107.94 (9)H4B—C4—H4A108.3
C2—N2—H2NB113.3 (11)N5—C5—C6109.89 (13)
Mn1—N2—H2NB109.1 (11)N5—C5—H5B109.7
C2—N2—H2NA109.1 (11)C6—C5—H5B109.7
Mn1—N2—H2NA109.2 (11)N5—C5—H5A109.7
H2NB—N2—H2NA108.0 (16)C6—C5—H5A109.7
C3—N3—Mn1109.61 (8)H5B—C5—H5A108.2
C3—N3—H3NB109.1 (11)N6—C6—C5109.25 (12)
Mn1—N3—H3NB108.6 (11)N6—C6—H6B109.8
C3—N3—H3NA111.5 (11)C5—C6—H6B109.8
Mn1—N3—H3NA111.0 (11)N6—C6—H6A109.8
H3NB—N3—H3NA106.9 (15)C5—C6—H6A109.8
C4—N4—Mn1107.12 (8)H6B—C6—H6A108.3
C4—N4—H4NB111.1 (11)C8—C7—H7A109.5
Mn1—N4—H4NB117.6 (11)C8—C7—H7B109.5
C4—N4—H4NA106.7 (11)H7A—C7—H7B109.5
Mn1—N4—H4NA106.3 (11)C8—C7—H7C109.5
H4NB—N4—H4NA107.4 (16)H7A—C7—H7C109.5
C5—N5—Mn1107.05 (10)H7B—C7—H7C109.5
C5—N5—H5NB109.9 (12)O2—C8—O1124.20 (14)
Mn1—N5—H5NB111.9 (12)O2—C8—C7118.61 (14)
C5—N5—H5NA110.1 (12)O1—C8—C7117.18 (14)
Mn1—N5—H5NA109.7 (12)C9—C10—H10A109.5
H5NB—N5—H5NA108.1 (17)C9—C10—H10B109.5
C6—N6—Mn1108.52 (10)H10A—C10—H10B109.5
C6—N6—H6NB109.5 (13)C9—C10—H10C109.5
Mn1—N6—H6NB111.4 (12)H10A—C10—H10C109.5
C6—N6—H6NA110.8 (12)H10B—C10—H10C109.5
Mn1—N6—H6NA109.8 (12)O3—C9—O4125.15 (15)
H6NB—N6—H6NA106.8 (17)O3—C9—C10117.53 (15)
N1—C1—C2108.81 (12)O4—C9—C10117.32 (15)
N1—C1—H1B109.9
N3—Mn1—N1—C149.3 (3)N1—Mn1—N5—C580.60 (10)
N5—Mn1—N1—C1176.20 (11)N3—Mn1—N5—C5106.24 (9)
N2—Mn1—N1—C117.47 (10)N2—Mn1—N5—C528.8 (2)
N6—Mn1—N1—C1105.90 (11)N6—Mn1—N5—C517.58 (9)
N4—Mn1—N1—C174.67 (10)N4—Mn1—N5—C5175.94 (9)
N1—Mn1—N2—C213.44 (10)N1—Mn1—N6—C6102.66 (10)
N3—Mn1—N2—C2174.51 (10)N3—Mn1—N6—C680.92 (10)
N5—Mn1—N2—C240.0 (2)N5—Mn1—N6—C612.87 (10)
N6—Mn1—N2—C285.03 (10)N2—Mn1—N6—C6179.44 (10)
N4—Mn1—N2—C2107.81 (10)N4—Mn1—N6—C674.9 (2)
N1—Mn1—N3—C316.5 (4)Mn1—N1—C1—C245.50 (15)
N5—Mn1—N3—C3110.19 (10)Mn1—N2—C2—C141.87 (15)
N2—Mn1—N3—C381.93 (9)N1—C1—C2—N260.16 (17)
N6—Mn1—N3—C3172.06 (10)Mn1—N3—C3—C438.03 (13)
N4—Mn1—N3—C39.36 (9)Mn1—N4—C4—C347.82 (13)
N1—Mn1—N4—C4162.87 (9)N3—C3—C4—N459.09 (16)
N3—Mn1—N4—C420.87 (9)Mn1—N5—C5—C645.71 (15)
N5—Mn1—N4—C470.29 (10)Mn1—N6—C6—C541.12 (15)
N2—Mn1—N4—C4118.92 (9)N5—C5—C6—N660.23 (18)
N6—Mn1—N4—C414.7 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1NB···O40.88 (1)2.07 (1)2.9413 (18)171 (2)
N1—H1NA···O4i0.87 (1)2.36 (1)3.0600 (17)138 (1)
N2—H2NB···O1ii0.87 (1)2.18 (1)3.0169 (16)160 (2)
N2—H2NA···O1iii0.87 (1)2.15 (1)3.0050 (18)167 (2)
N3—H3NB···O20.86 (1)2.11 (1)2.9638 (18)172 (2)
N3—H3NA···O2ii0.87 (1)2.23 (1)3.0677 (18)162 (2)
N4—H4NB···O3iv0.87 (1)2.17 (1)2.9839 (16)157 (2)
N4—H4NA···O1iii0.87 (1)2.19 (1)3.0392 (18)167 (2)
N5—H5NB···O20.87 (1)2.44 (1)3.215 (2)149 (2)
N5—H5NA···O4i0.87 (1)2.12 (1)2.9408 (17)157 (2)
N6—H6NB···O30.87 (1)2.07 (1)2.9366 (19)171 (2)
N6—H6NA···O2ii0.87 (1)2.83 (1)3.619 (2)152 (2)
Symmetry codes: (i) x+1, y+1, z+2; (ii) x+1, y+1, z+1; (iii) x, y+1, z; (iv) x+1, y, z.
Tris(ethylenediamine-κ2N,N')iron(II) diacetate (umd815) top
Crystal data top
[Fe(C2H8N2)3](C2H3O2)2Z = 2
Mr = 354.25F(000) = 380
Triclinic, P1Dx = 1.320 Mg m3
a = 8.3426 (9) ÅCu Kα radiation, λ = 1.54178 Å
b = 9.1332 (10) ÅCell parameters from 8016 reflections
c = 12.8165 (14) Åθ = 6.5–68.4°
α = 70.423 (5)°µ = 7.00 mm1
β = 86.074 (4)°T = 200 K
γ = 75.628 (5)°Plate, yellow
V = 891.19 (17) Å30.20 × 0.17 × 0.14 mm
Data collection top
Bruker CMOS
diffractometer
3214 independent reflections
Radiation source: fine-focus sealed tube2950 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
φ and ω scansθmax = 68.4°, θmin = 6.5°
Absorption correction: multi-scan
(SADABS; Bruker, 2014)
h = 109
Tmin = 0.335, Tmax = 0.441k = 1111
11719 measured reflectionsl = 1515
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)] = 0.032H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.080 w = 1/[σ2(Fo2) + (0.0329P)2 + 0.4027P]
where P = (Fo2 + 2Fc2)/3
S = 1.04(Δ/σ)max = 0.032
3214 reflectionsΔρmax = 0.32 e Å3
229 parametersΔρmin = 0.23 e Å3
12 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0020 (8)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Fe10.56462 (4)0.64380 (4)0.71347 (2)0.02355 (13)
O10.7351 (2)0.0421 (2)0.55820 (14)0.0461 (4)
O20.7073 (3)0.2747 (2)0.5798 (2)0.0712 (7)
O30.0632 (2)0.6747 (3)0.85454 (14)0.0547 (5)
O40.23459 (19)0.6196 (2)0.99416 (13)0.0458 (4)
N10.5317 (2)0.6918 (2)0.87072 (14)0.0313 (4)
H1NB0.449 (2)0.657 (3)0.9074 (18)0.038*
H1NA0.618 (2)0.638 (3)0.9148 (17)0.038*
N20.4475 (2)0.9036 (2)0.65327 (14)0.0312 (4)
H2NB0.371 (2)0.923 (3)0.6046 (16)0.037*
H2NA0.522 (2)0.956 (3)0.6227 (19)0.037*
N30.6223 (2)0.6197 (2)0.54856 (13)0.0271 (4)
H3NB0.633 (3)0.5203 (14)0.5531 (19)0.033*
H3NA0.540 (2)0.675 (2)0.5037 (16)0.033*
N40.8175 (2)0.6856 (2)0.69066 (15)0.0316 (4)
H4NB0.882 (3)0.653 (3)0.7488 (14)0.038*
H4NA0.806 (3)0.7891 (13)0.6636 (19)0.038*
N50.6332 (3)0.3822 (2)0.79907 (15)0.0361 (4)
H5NB0.688 (3)0.330 (3)0.7572 (19)0.043*
H5NA0.696 (3)0.360 (3)0.8563 (15)0.043*
N60.3246 (2)0.5854 (3)0.70608 (15)0.0377 (4)
H6NB0.250 (2)0.621 (3)0.7476 (19)0.045*
H6NA0.284 (3)0.632 (3)0.6388 (11)0.045*
C10.5033 (3)0.8651 (3)0.84614 (18)0.0404 (5)
H1B0.60880.89820.82610.048*
H1A0.45940.89420.91210.048*
C20.3798 (3)0.9493 (3)0.75037 (19)0.0404 (5)
H2A0.27350.91810.77130.049*
H2B0.35901.06670.73220.049*
C30.7750 (3)0.6713 (3)0.50936 (16)0.0322 (5)
H3B0.74970.78930.47630.039*
H3A0.82470.62490.45160.039*
C40.8964 (3)0.6167 (3)0.60555 (18)0.0353 (5)
H4B0.92600.49840.63680.042*
H4A0.99890.65340.57990.042*
C50.4770 (3)0.3326 (3)0.83203 (19)0.0447 (6)
H5B0.43210.36360.89710.054*
H5A0.49790.21480.85300.054*
C60.3530 (3)0.4113 (3)0.73725 (18)0.0422 (6)
H6B0.39550.37670.67310.051*
H6A0.24760.37910.75990.051*
C70.9463 (3)0.0730 (3)0.6558 (2)0.0519 (7)
H7A0.97150.15790.67790.078*
H7B1.03400.03880.60810.078*
H7C0.93940.01820.72200.078*
C80.7829 (2)0.1357 (2)0.59342 (16)0.0284 (4)
C90.0950 (3)0.6731 (3)0.94795 (17)0.0348 (5)
C100.0470 (4)0.7411 (5)1.0117 (3)0.0682 (9)
H10A0.11990.66731.03700.102*
H10B0.10970.84490.96340.102*
H10C0.00310.75501.07580.102*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.02226 (18)0.02674 (19)0.02107 (17)0.00375 (12)0.00380 (11)0.00786 (12)
O10.0535 (10)0.0392 (9)0.0489 (10)0.0160 (8)0.0171 (8)0.0117 (8)
O20.0661 (13)0.0420 (11)0.1055 (17)0.0181 (10)0.0449 (12)0.0377 (11)
O30.0418 (10)0.0879 (14)0.0347 (9)0.0142 (10)0.0100 (7)0.0197 (9)
O40.0317 (9)0.0655 (11)0.0340 (8)0.0041 (8)0.0104 (7)0.0118 (8)
N10.0324 (10)0.0361 (10)0.0229 (8)0.0028 (8)0.0052 (7)0.0092 (8)
N20.0312 (10)0.0302 (9)0.0285 (9)0.0024 (8)0.0098 (7)0.0065 (7)
N30.0249 (9)0.0311 (9)0.0254 (8)0.0041 (7)0.0046 (7)0.0102 (7)
N40.0260 (9)0.0363 (10)0.0323 (9)0.0047 (8)0.0090 (7)0.0111 (8)
N50.0471 (12)0.0304 (10)0.0289 (9)0.0045 (9)0.0112 (8)0.0082 (8)
N60.0303 (10)0.0547 (12)0.0290 (9)0.0129 (9)0.0009 (8)0.0126 (9)
C10.0521 (14)0.0395 (13)0.0335 (11)0.0062 (11)0.0066 (10)0.0192 (10)
C20.0433 (13)0.0341 (12)0.0410 (12)0.0043 (10)0.0055 (10)0.0171 (10)
C30.0298 (11)0.0406 (12)0.0265 (10)0.0073 (9)0.0022 (8)0.0128 (9)
C40.0218 (10)0.0428 (13)0.0410 (12)0.0032 (9)0.0017 (9)0.0163 (10)
C50.0667 (17)0.0435 (14)0.0290 (11)0.0269 (13)0.0007 (11)0.0084 (10)
C60.0490 (14)0.0564 (15)0.0331 (11)0.0288 (12)0.0017 (10)0.0186 (11)
C70.0375 (13)0.0427 (14)0.0699 (18)0.0077 (11)0.0226 (12)0.0080 (13)
C80.0259 (10)0.0286 (11)0.0287 (10)0.0071 (9)0.0008 (8)0.0063 (8)
C90.0305 (11)0.0415 (12)0.0289 (11)0.0094 (10)0.0039 (9)0.0058 (9)
C100.0424 (16)0.095 (2)0.0633 (18)0.0005 (16)0.0047 (13)0.0341 (18)
Geometric parameters (Å, º) top
Fe1—N12.1880 (17)N6—H6NB0.867 (10)
Fe1—N32.2062 (16)N6—H6NA0.871 (10)
Fe1—N52.2115 (19)C1—C21.519 (3)
Fe1—N62.2124 (18)C1—H1B0.9900
Fe1—N22.2147 (18)C1—H1A0.9900
Fe1—N42.2183 (18)C2—H2A0.9900
O1—C81.244 (2)C2—H2B0.9900
O2—C81.228 (3)C3—C41.518 (3)
O3—C91.239 (3)C3—H3B0.9900
O4—C91.250 (3)C3—H3A0.9900
N1—C11.466 (3)C4—H4B0.9900
N1—H1NB0.871 (10)C4—H4A0.9900
N1—H1NA0.878 (10)C5—C61.510 (4)
N2—C21.475 (3)C5—H5B0.9900
N2—H2NB0.871 (10)C5—H5A0.9900
N2—H2NA0.867 (10)C6—H6B0.9900
N3—C31.466 (3)C6—H6A0.9900
N3—H3NB0.872 (10)C7—C81.510 (3)
N3—H3NA0.865 (10)C7—H7A0.9800
N4—C41.475 (3)C7—H7B0.9800
N4—H4NB0.870 (10)C7—H7C0.9800
N4—H4NA0.874 (10)C9—C101.516 (4)
N5—C51.474 (3)C10—H10A0.9800
N5—H5NB0.872 (10)C10—H10B0.9800
N5—H5NA0.870 (10)C10—H10C0.9800
N6—C61.464 (3)
N1—Fe1—N3171.55 (7)C2—C1—H1B110.0
N1—Fe1—N591.93 (7)N1—C1—H1A110.0
N3—Fe1—N593.16 (7)C2—C1—H1A110.0
N1—Fe1—N698.38 (7)H1B—C1—H1A108.4
N3—Fe1—N689.16 (6)N2—C2—C1109.03 (18)
N5—Fe1—N679.85 (8)N2—C2—H2A109.9
N1—Fe1—N279.84 (7)C1—C2—H2A109.9
N3—Fe1—N296.26 (7)N2—C2—H2B109.9
N5—Fe1—N2166.99 (7)C1—C2—H2B109.9
N6—Fe1—N291.31 (7)H2A—C2—H2B108.3
N1—Fe1—N493.38 (7)N3—C3—C4109.66 (17)
N3—Fe1—N479.23 (6)N3—C3—H3B109.7
N5—Fe1—N498.21 (7)C4—C3—H3B109.7
N6—Fe1—N4168.13 (7)N3—C3—H3A109.7
N2—Fe1—N492.37 (7)C4—C3—H3A109.7
C1—N1—Fe1107.91 (13)H3B—C3—H3A108.2
C1—N1—H1NB110.4 (17)N4—C4—C3108.27 (17)
Fe1—N1—H1NB111.5 (16)N4—C4—H4B110.0
C1—N1—H1NA112.2 (16)C3—C4—H4B110.0
Fe1—N1—H1NA110.7 (16)N4—C4—H4A110.0
H1NB—N1—H1NA104 (2)C3—C4—H4A110.0
C2—N2—Fe1107.38 (13)H4B—C4—H4A108.4
C2—N2—H2NB111.8 (17)N5—C5—C6109.93 (18)
Fe1—N2—H2NB109.3 (17)N5—C5—H5B109.7
C2—N2—H2NA109.4 (16)C6—C5—H5B109.7
Fe1—N2—H2NA109.5 (17)N5—C5—H5A109.7
H2NB—N2—H2NA109 (2)C6—C5—H5A109.7
C3—N3—Fe1109.12 (12)H5B—C5—H5A108.2
C3—N3—H3NB111.0 (16)N6—C6—C5109.20 (18)
Fe1—N3—H3NB109.2 (16)N6—C6—H6B109.8
C3—N3—H3NA112.1 (16)C5—C6—H6B109.8
Fe1—N3—H3NA109.4 (16)N6—C6—H6A109.8
H3NB—N3—H3NA106 (2)C5—C6—H6A109.8
C4—N4—Fe1106.94 (12)H6B—C6—H6A108.3
C4—N4—H4NB110.9 (17)C8—C7—H7A109.5
Fe1—N4—H4NB118.2 (17)C8—C7—H7B109.5
C4—N4—H4NA107.6 (17)H7A—C7—H7B109.5
Fe1—N4—H4NA106.9 (17)C8—C7—H7C109.5
H4NB—N4—H4NA106 (2)H7A—C7—H7C109.5
C5—N5—Fe1106.44 (15)H7B—C7—H7C109.5
C5—N5—H5NB109.6 (17)O2—C8—O1124.5 (2)
Fe1—N5—H5NB112.8 (18)O2—C8—C7118.5 (2)
C5—N5—H5NA111.5 (17)O1—C8—C7117.1 (2)
Fe1—N5—H5NA109.9 (18)O3—C9—O4125.4 (2)
H5NB—N5—H5NA107 (3)O3—C9—C10117.3 (2)
C6—N6—Fe1108.31 (14)O4—C9—C10117.3 (2)
C6—N6—H6NB110.3 (18)C9—C10—H10A109.5
Fe1—N6—H6NB113.6 (17)C9—C10—H10B109.5
C6—N6—H6NA110.4 (18)H10A—C10—H10B109.5
Fe1—N6—H6NA108.9 (18)C9—C10—H10C109.5
H6NB—N6—H6NA105 (3)H10A—C10—H10C109.5
N1—C1—C2108.50 (17)H10B—C10—H10C109.5
N1—C1—H1B110.0
N3—Fe1—N1—C145.7 (5)N1—Fe1—N5—C580.71 (14)
N5—Fe1—N1—C1172.82 (15)N3—Fe1—N5—C5106.03 (13)
N6—Fe1—N1—C1107.15 (15)N6—Fe1—N5—C517.46 (13)
N2—Fe1—N1—C117.32 (14)N2—Fe1—N5—C530.4 (3)
N4—Fe1—N1—C174.48 (15)N4—Fe1—N5—C5174.41 (13)
N1—Fe1—N2—C213.39 (14)N1—Fe1—N6—C6102.80 (14)
N3—Fe1—N2—C2174.18 (14)N3—Fe1—N6—C681.04 (14)
N5—Fe1—N2—C238.0 (3)N5—Fe1—N6—C612.32 (13)
N6—Fe1—N2—C284.89 (14)N2—Fe1—N6—C6177.29 (14)
N4—Fe1—N2—C2106.40 (14)N4—Fe1—N6—C669.2 (4)
N1—Fe1—N3—C319.4 (5)Fe1—N1—C1—C244.9 (2)
N5—Fe1—N3—C3107.63 (14)Fe1—N2—C2—C141.5 (2)
N6—Fe1—N3—C3172.58 (14)N1—C1—C2—N259.4 (2)
N2—Fe1—N3—C381.36 (14)Fe1—N3—C3—C438.3 (2)
N4—Fe1—N3—C39.87 (14)Fe1—N4—C4—C346.80 (19)
N1—Fe1—N4—C4163.81 (14)N3—C3—C4—N458.4 (2)
N3—Fe1—N4—C420.32 (14)Fe1—N5—C5—C644.8 (2)
N5—Fe1—N4—C471.36 (14)Fe1—N6—C6—C539.9 (2)
N6—Fe1—N4—C48.3 (4)N5—C5—C6—N658.7 (3)
N2—Fe1—N4—C4116.24 (14)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1NB···O40.87 (1)2.08 (1)2.942 (2)169 (2)
N1—H1NA···O4i0.88 (1)2.31 (2)3.050 (3)142 (2)
N2—H2NB···O1ii0.87 (1)2.21 (1)3.033 (2)157 (2)
N2—H2NA···O1iii0.87 (1)2.13 (1)2.986 (3)169 (2)
N3—H3NB···O20.87 (1)2.09 (1)2.945 (3)168 (2)
N3—H3NA···O2ii0.87 (1)2.26 (1)3.072 (3)157 (2)
N4—H4NB···O3iv0.87 (1)2.19 (1)2.995 (2)154 (2)
N4—H4NA···O1iii0.87 (1)2.20 (1)3.050 (3)163 (2)
N5—H5NB···O20.87 (1)2.47 (2)3.249 (3)148 (2)
N5—H5NA···O4i0.87 (1)2.12 (1)2.933 (2)156 (2)
N6—H6NB···O30.87 (1)2.08 (1)2.938 (3)172 (2)
N6—H6NA···O2ii0.87 (1)2.64 (2)3.457 (3)156 (2)
Symmetry codes: (i) x+1, y+1, z+2; (ii) x+1, y+1, z+1; (iii) x, y+1, z; (iv) x+1, y, z.
Tris(ethylenediamine-κ2N,N')cobalt(II) diacetate (umd906_a) top
Crystal data top
[Co(C2H8N2)3](C2H3O2)2Z = 2
Mr = 357.33F(000) = 382
Triclinic, P1Dx = 1.347 Mg m3
a = 8.3029 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.1295 (10) ÅCell parameters from 9939 reflections
c = 12.7175 (13) Åθ = 3.0–25.4°
α = 71.021 (4)°µ = 1.00 mm1
β = 85.776 (4)°T = 200 K
γ = 75.146 (4)°Plate, pink
V = 881.09 (16) Å30.18 × 0.14 × 0.08 mm
Data collection top
Bruker CMOS
diffractometer
3228 independent reflections
Radiation source: fine-focus sealed tube2900 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.029
φ and ω scansθmax = 25.4°, θmin = 3.0°
Absorption correction: multi-scan
(SADABS; Bruker, 2014)
h = 1010
Tmin = 0.841, Tmax = 0.925k = 1111
18117 measured reflectionsl = 1515
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)] = 0.023H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.056 w = 1/[σ2(Fo2) + (0.0197P)2 + 0.429P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.008
3228 reflectionsΔρmax = 0.25 e Å3
229 parametersΔρmin = 0.21 e Å3
12 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0150 (15)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Co10.56421 (3)0.64621 (2)0.713098 (17)0.02053 (9)
O10.73486 (17)0.04297 (15)0.55755 (11)0.0405 (3)
O20.7130 (2)0.27882 (17)0.57473 (15)0.0600 (5)
N10.52793 (18)0.68921 (17)0.87030 (11)0.0275 (3)
H1NB0.4410 (17)0.659 (2)0.9046 (14)0.033*
H1NA0.6129 (17)0.6345 (19)0.9138 (13)0.033*
N20.45016 (18)0.90141 (17)0.65411 (12)0.0268 (3)
H2NB0.3718 (18)0.923 (2)0.6051 (13)0.032*
H2NA0.5221 (19)0.957 (2)0.6225 (14)0.032*
N30.62086 (17)0.62139 (16)0.55011 (11)0.0226 (3)
H3NB0.638 (2)0.5223 (12)0.5551 (15)0.027*
H3NA0.5374 (17)0.6736 (19)0.5054 (13)0.027*
N40.81262 (17)0.68843 (17)0.69260 (12)0.0268 (3)
H4NB0.874 (2)0.656 (2)0.7517 (11)0.032*
H4NA0.800 (2)0.7913 (12)0.6651 (15)0.032*
N50.6378 (2)0.38943 (17)0.79340 (12)0.0304 (3)
H5NB0.690 (2)0.340 (2)0.7486 (14)0.037*
H5NA0.702 (2)0.369 (2)0.8493 (12)0.037*
N60.32640 (18)0.59151 (19)0.70741 (12)0.0314 (3)
H6NB0.254 (2)0.622 (2)0.7542 (14)0.038*
H6NA0.285 (2)0.639 (2)0.6404 (10)0.038*
C10.5010 (2)0.8621 (2)0.84870 (15)0.0347 (4)
H1B0.60810.89330.83070.042*
H1A0.45480.89060.91550.042*
C20.3799 (2)0.9491 (2)0.75155 (15)0.0353 (4)
H2A0.27140.92140.77090.042*
H2B0.36151.06610.73420.042*
C30.7745 (2)0.6728 (2)0.50995 (14)0.0276 (4)
H3B0.74850.79060.47690.033*
H3A0.82540.62520.45190.033*
C40.8951 (2)0.6190 (2)0.60690 (15)0.0305 (4)
H4B0.92590.50090.63770.037*
H4A0.99790.65580.58180.037*
C50.4837 (3)0.3360 (2)0.82819 (15)0.0381 (4)
H5B0.44000.36320.89580.046*
H5A0.50730.21860.84590.046*
C60.3556 (2)0.4173 (2)0.73516 (15)0.0363 (4)
H6B0.39640.38480.66890.044*
H6A0.25020.38490.75880.044*
C70.9476 (2)0.0721 (2)0.65648 (19)0.0458 (5)
H7A0.97460.15740.67730.069*
H7B1.03670.03250.61030.069*
H7C0.93690.01560.72380.069*
C80.7854 (2)0.13658 (19)0.59199 (13)0.0246 (3)
O30.05832 (17)0.67811 (19)0.85660 (11)0.0479 (4)
O40.23078 (15)0.61838 (17)0.99746 (10)0.0402 (3)
C100.0528 (3)0.7413 (3)1.0172 (2)0.0632 (7)
H10A0.12480.83840.96770.095*
H10B0.00830.76701.07650.095*
H10C0.11770.66181.05000.095*
C90.0899 (2)0.6742 (2)0.95136 (14)0.0315 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co10.02004 (13)0.02428 (13)0.01723 (12)0.00393 (8)0.00400 (8)0.00682 (8)
O10.0486 (8)0.0350 (7)0.0414 (8)0.0166 (6)0.0161 (6)0.0084 (6)
O20.0594 (10)0.0357 (8)0.0842 (12)0.0139 (7)0.0370 (9)0.0297 (8)
N10.0287 (8)0.0317 (8)0.0205 (7)0.0035 (6)0.0049 (6)0.0082 (6)
N20.0277 (8)0.0274 (7)0.0233 (7)0.0025 (6)0.0085 (6)0.0066 (6)
N30.0213 (7)0.0259 (7)0.0208 (7)0.0038 (6)0.0042 (5)0.0085 (6)
N40.0238 (7)0.0304 (7)0.0268 (8)0.0055 (6)0.0081 (6)0.0090 (6)
N50.0402 (9)0.0278 (8)0.0232 (8)0.0057 (6)0.0096 (6)0.0079 (6)
N60.0270 (8)0.0469 (9)0.0226 (8)0.0125 (7)0.0016 (6)0.0113 (7)
C10.0446 (11)0.0347 (10)0.0277 (9)0.0050 (8)0.0059 (8)0.0160 (8)
C20.0375 (10)0.0315 (9)0.0334 (10)0.0040 (8)0.0057 (8)0.0141 (8)
C30.0251 (9)0.0340 (9)0.0248 (9)0.0076 (7)0.0022 (7)0.0110 (7)
C40.0202 (8)0.0371 (9)0.0345 (10)0.0041 (7)0.0020 (7)0.0134 (8)
C50.0592 (13)0.0370 (10)0.0230 (9)0.0255 (9)0.0009 (8)0.0055 (8)
C60.0443 (11)0.0498 (11)0.0265 (9)0.0273 (9)0.0029 (8)0.0164 (8)
C70.0370 (11)0.0374 (11)0.0596 (14)0.0077 (8)0.0218 (10)0.0072 (10)
C80.0228 (8)0.0268 (9)0.0234 (8)0.0072 (7)0.0012 (6)0.0059 (7)
O30.0361 (8)0.0806 (11)0.0283 (7)0.0124 (7)0.0087 (6)0.0184 (7)
O40.0287 (7)0.0599 (9)0.0282 (7)0.0073 (6)0.0084 (5)0.0099 (6)
C100.0403 (13)0.0936 (19)0.0538 (14)0.0018 (12)0.0042 (11)0.0329 (14)
C90.0274 (9)0.0389 (10)0.0254 (9)0.0093 (7)0.0032 (7)0.0050 (7)
Geometric parameters (Å, º) top
Co1—N12.1455 (14)C1—H1B0.9900
Co1—N22.1735 (14)C1—H1A0.9900
Co1—N32.1625 (13)C1—C21.518 (2)
Co1—N42.1757 (14)C2—H2A0.9900
Co1—N52.1708 (15)C2—H2B0.9900
Co1—N62.1687 (15)C3—H3B0.9900
O1—C81.2460 (19)C3—H3A0.9900
O2—C81.237 (2)C3—C41.517 (2)
N1—H1NB0.874 (9)C4—H4B0.9900
N1—H1NA0.866 (9)C4—H4A0.9900
N1—C11.471 (2)C5—H5B0.9900
N2—H2NB0.874 (9)C5—H5A0.9900
N2—H2NA0.871 (9)C5—C61.514 (3)
N2—C21.476 (2)C6—H6B0.9900
N3—H3NB0.861 (9)C6—H6A0.9900
N3—H3NA0.862 (9)C7—H7A0.9800
N3—C31.471 (2)C7—H7B0.9800
N4—H4NB0.864 (9)C7—H7C0.9800
N4—H4NA0.870 (9)C7—C81.508 (2)
N4—C41.475 (2)O3—C91.239 (2)
N5—H5NB0.863 (9)O4—C91.254 (2)
N5—H5NA0.865 (9)C10—H10A0.9800
N5—C51.472 (2)C10—H10B0.9800
N6—H6NB0.875 (9)C10—H10C0.9800
N6—H6NA0.870 (9)C10—C91.515 (3)
N6—C61.471 (2)
N1—Co1—N281.10 (5)N1—C1—C2108.29 (14)
N1—Co1—N3173.17 (5)H1B—C1—H1A108.4
N1—Co1—N493.52 (6)C2—C1—H1B110.0
N1—Co1—N591.80 (6)C2—C1—H1A110.0
N1—Co1—N696.53 (6)N2—C2—C1108.83 (14)
N2—Co1—N491.32 (6)N2—C2—H2A109.9
N3—Co1—N295.85 (5)N2—C2—H2B109.9
N3—Co1—N480.39 (5)C1—C2—H2A109.9
N3—Co1—N592.06 (5)C1—C2—H2B109.9
N3—Co1—N689.64 (5)H2A—C2—H2B108.3
N5—Co1—N2169.01 (6)N3—C3—H3B109.9
N5—Co1—N497.53 (6)N3—C3—H3A109.9
N6—Co1—N291.42 (6)N3—C3—C4108.98 (13)
N6—Co1—N4169.88 (5)H3B—C3—H3A108.3
N6—Co1—N581.00 (6)C4—C3—H3B109.9
Co1—N1—H1NB111.6 (13)C4—C3—H3A109.9
Co1—N1—H1NA110.3 (13)N4—C4—C3108.07 (13)
H1NB—N1—H1NA106.5 (18)N4—C4—H4B110.1
C1—N1—Co1107.67 (10)N4—C4—H4A110.1
C1—N1—H1NB108.8 (12)C3—C4—H4B110.1
C1—N1—H1NA112.1 (12)C3—C4—H4A110.1
Co1—N2—H2NB110.6 (12)H4B—C4—H4A108.4
Co1—N2—H2NA112.0 (13)N5—C5—H5B109.8
H2NB—N2—H2NA107.4 (18)N5—C5—H5A109.8
C2—N2—Co1107.44 (10)N5—C5—C6109.29 (14)
C2—N2—H2NB110.4 (13)H5B—C5—H5A108.3
C2—N2—H2NA109.0 (12)C6—C5—H5B109.8
Co1—N3—H3NB109.1 (12)C6—C5—H5A109.8
Co1—N3—H3NA110.4 (12)N6—C6—C5109.08 (14)
H3NB—N3—H3NA107.3 (17)N6—C6—H6B109.9
C3—N3—Co1109.16 (9)N6—C6—H6A109.9
C3—N3—H3NB108.0 (12)C5—C6—H6B109.9
C3—N3—H3NA112.8 (12)C5—C6—H6A109.9
Co1—N4—H4NB117.2 (13)H6B—C6—H6A108.3
Co1—N4—H4NA106.7 (13)H7A—C7—H7B109.5
H4NB—N4—H4NA107.2 (17)H7A—C7—H7C109.5
C4—N4—Co1106.73 (10)H7B—C7—H7C109.5
C4—N4—H4NB111.5 (13)C8—C7—H7A109.5
C4—N4—H4NA107.0 (13)C8—C7—H7B109.5
Co1—N5—H5NB111.9 (13)C8—C7—H7C109.5
Co1—N5—H5NA108.7 (13)O1—C8—C7117.42 (15)
H5NB—N5—H5NA109.1 (19)O2—C8—O1124.27 (16)
C5—N5—Co1106.95 (11)O2—C8—C7118.30 (15)
C5—N5—H5NB108.2 (13)H10A—C10—H10B109.5
C5—N5—H5NA112.0 (13)H10A—C10—H10C109.5
Co1—N6—H6NB113.5 (13)H10B—C10—H10C109.5
Co1—N6—H6NA108.5 (13)C9—C10—H10A109.5
H6NB—N6—H6NA108.8 (19)C9—C10—H10B109.5
C6—N6—Co1108.10 (11)C9—C10—H10C109.5
C6—N6—H6NB108.1 (13)O3—C9—O4125.14 (17)
C6—N6—H6NA109.9 (13)O3—C9—C10117.61 (17)
N1—C1—H1B110.0O4—C9—C10117.25 (17)
N1—C1—H1A110.0
Co1—N1—C1—C244.81 (16)N3—Co1—N5—C5106.27 (11)
Co1—N2—C2—C140.46 (17)N3—Co1—N6—C679.47 (11)
Co1—N3—C3—C437.93 (15)N3—C3—C4—N457.83 (17)
Co1—N4—C4—C346.87 (15)N4—Co1—N1—C173.08 (12)
Co1—N5—C5—C643.75 (16)N4—Co1—N2—C2106.02 (11)
Co1—N6—C6—C539.93 (16)N4—Co1—N3—C39.67 (10)
N1—Co1—N2—C212.67 (11)N4—Co1—N5—C5173.15 (11)
N1—Co1—N3—C317.5 (5)N4—Co1—N6—C669.7 (4)
N1—Co1—N4—C4162.61 (11)N5—Co1—N1—C1170.74 (11)
N1—Co1—N5—C579.36 (11)N5—Co1—N2—C237.6 (3)
N1—Co1—N6—C6103.48 (11)N5—Co1—N3—C3106.96 (11)
N1—C1—C2—N258.3 (2)N5—Co1—N4—C470.32 (11)
N2—Co1—N1—C117.70 (11)N5—Co1—N6—C612.68 (11)
N2—Co1—N3—C380.67 (11)N5—C5—C6—N657.53 (19)
N2—Co1—N4—C4116.23 (11)N6—Co1—N1—C1108.12 (12)
N2—Co1—N5—C529.8 (3)N6—Co1—N2—C283.72 (11)
N2—Co1—N6—C6175.31 (11)N6—Co1—N3—C3172.06 (11)
N3—Co1—N1—C146.3 (5)N6—Co1—N4—C410.6 (4)
N3—Co1—N2—C2173.50 (11)N6—Co1—N5—C516.96 (11)
N3—Co1—N4—C420.51 (10)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1NB···O40.87 (1)2.08 (1)2.945 (2)170 (2)
N1—H1NA···O4i0.87 (1)2.30 (1)3.0443 (19)145 (2)
N2—H2NB···O1ii0.87 (1)2.21 (1)3.0305 (18)157 (2)
N2—H2NA···O1iii0.87 (1)2.12 (1)2.979 (2)168 (2)
N3—H3NB···O20.86 (1)2.08 (1)2.9387 (19)172 (2)
N3—H3NA···O2ii0.86 (1)2.26 (1)3.074 (2)157 (2)
N4—H4NB···O3iv0.86 (1)2.19 (1)2.9868 (18)153 (2)
N4—H4NA···O1iii0.87 (1)2.21 (1)3.053 (2)164 (2)
N5—H5NB···O20.86 (1)2.44 (1)3.223 (2)152 (2)
N5—H5NA···O4i0.87 (1)2.11 (1)2.9215 (19)156 (2)
N6—H6NB···O30.88 (1)2.07 (1)2.938 (2)171 (2)
N6—H6NA···O2ii0.87 (1)2.59 (1)3.405 (2)156 (2)
Symmetry codes: (i) x+1, y+1, z+2; (ii) x+1, y+1, z+1; (iii) x, y+1, z; (iv) x+1, y, z.
Tris(ethylenediamine-κ2N,N')nickel(II) diacetate (umd908) top
Crystal data top
[Ni(C2H8N2)3](C2H3O2)2Z = 2
Mr = 357.11F(000) = 384
Triclinic, P1Dx = 1.367 Mg m3
a = 8.2974 (11) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.0619 (11) ÅCell parameters from 9139 reflections
c = 12.5998 (17) Åθ = 3.1–25.4°
α = 71.960 (4)°µ = 1.14 mm1
β = 85.204 (5)°T = 200 K
γ = 74.321 (4)°Block, green
V = 867.29 (19) Å30.21 × 0.17 × 0.12 mm
Data collection top
Bruker CMOS
diffractometer
3175 independent reflections
Radiation source: fine-focus sealed tube3010 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.028
φ and ω scansθmax = 25.4°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2014)
h = 1010
Tmin = 0.796, Tmax = 0.875k = 1010
25372 measured reflectionsl = 1515
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)] = 0.019H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.049 w = 1/[σ2(Fo2) + (0.0185P)2 + 0.4044P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max = 0.015
3175 reflectionsΔρmax = 0.27 e Å3
229 parametersΔρmin = 0.23 e Å3
12 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.027 (2)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Ni10.56174 (2)0.647713 (19)0.713433 (13)0.01785 (8)
O10.72555 (16)0.04539 (14)0.56195 (10)0.0416 (3)
O20.72642 (17)0.28635 (14)0.56539 (12)0.0507 (3)
N10.52299 (15)0.68764 (15)0.87080 (10)0.0248 (3)
H1NB0.4349 (15)0.6596 (19)0.9054 (13)0.030*
H1NA0.6106 (15)0.6347 (18)0.9116 (12)0.030*
N20.44608 (15)0.89785 (14)0.65675 (10)0.0248 (3)
H2NB0.3713 (17)0.9171 (19)0.6067 (11)0.030*
H2NA0.5188 (17)0.9520 (18)0.6269 (13)0.030*
N30.61690 (14)0.62791 (14)0.55076 (9)0.0207 (2)
H3NB0.6337 (19)0.5296 (12)0.5532 (13)0.025*
H3NA0.5344 (15)0.6849 (17)0.5061 (11)0.025*
N40.80561 (15)0.68763 (15)0.69738 (10)0.0253 (3)
H4NB0.8677 (18)0.6519 (19)0.7564 (10)0.030*
H4NA0.794 (2)0.7903 (11)0.6737 (14)0.030*
N50.64437 (16)0.39612 (14)0.78853 (10)0.0272 (3)
H5NB0.7007 (19)0.3480 (19)0.7423 (12)0.033*
H5NA0.7071 (19)0.378 (2)0.8447 (11)0.033*
N60.32979 (16)0.59221 (16)0.70824 (10)0.0278 (3)
H6NB0.2551 (18)0.624 (2)0.7544 (12)0.033*
H6NA0.288 (2)0.6388 (19)0.6413 (9)0.033*
C10.4927 (2)0.86129 (18)0.85209 (13)0.0326 (3)
H1B0.59930.89320.83470.039*
H1A0.44410.88950.91990.039*
C20.3721 (2)0.94759 (18)0.75489 (13)0.0334 (3)
H2A0.26370.91980.77390.040*
H2B0.35201.06530.73830.040*
C30.77221 (17)0.67664 (18)0.51149 (12)0.0262 (3)
H3B0.74710.79500.48000.031*
H3A0.82400.62850.45220.031*
C40.89155 (17)0.61997 (19)0.60919 (13)0.0290 (3)
H4B0.92340.50120.63740.035*
H4A0.99450.65690.58550.035*
C50.4936 (2)0.33721 (19)0.82477 (13)0.0349 (4)
H5B0.44930.36250.89430.042*
H5A0.52220.21920.84010.042*
C60.3629 (2)0.4170 (2)0.73365 (12)0.0328 (3)
H6B0.40360.38480.66590.039*
H6A0.25860.38320.75860.039*
C70.9475 (2)0.0684 (2)0.65631 (17)0.0456 (4)
H7A0.97770.15250.67780.068*
H7B1.03690.02380.61030.068*
H7C0.93250.01710.72350.068*
C80.78614 (17)0.13917 (16)0.59041 (11)0.0226 (3)
O30.05512 (15)0.68032 (17)0.85836 (9)0.0458 (3)
O40.22577 (13)0.61536 (15)1.00070 (9)0.0379 (3)
C100.0593 (2)0.7434 (3)1.02143 (18)0.0610 (6)
H10A0.12590.84600.97400.092*
H10B0.01570.76061.08530.092*
H10C0.12980.66821.04830.092*
C90.08530 (18)0.67426 (19)0.95450 (12)0.0294 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.01869 (11)0.02042 (11)0.01467 (10)0.00450 (7)0.00408 (6)0.00497 (7)
O10.0522 (7)0.0365 (6)0.0409 (7)0.0230 (5)0.0179 (6)0.0040 (5)
O20.0534 (8)0.0296 (6)0.0662 (9)0.0089 (5)0.0279 (7)0.0202 (6)
N10.0255 (6)0.0287 (6)0.0191 (6)0.0035 (5)0.0054 (5)0.0074 (5)
N20.0254 (6)0.0243 (6)0.0228 (6)0.0038 (5)0.0080 (5)0.0048 (5)
N30.0204 (6)0.0234 (6)0.0184 (6)0.0046 (5)0.0039 (4)0.0063 (5)
N40.0229 (6)0.0281 (6)0.0262 (6)0.0069 (5)0.0087 (5)0.0075 (5)
N50.0365 (7)0.0248 (6)0.0201 (6)0.0058 (5)0.0081 (5)0.0062 (5)
N60.0254 (6)0.0413 (7)0.0199 (6)0.0133 (5)0.0013 (5)0.0090 (5)
C10.0413 (9)0.0322 (8)0.0274 (8)0.0051 (7)0.0061 (7)0.0154 (6)
C20.0373 (9)0.0275 (8)0.0325 (8)0.0029 (6)0.0066 (7)0.0129 (6)
C30.0252 (7)0.0313 (8)0.0226 (7)0.0085 (6)0.0026 (6)0.0081 (6)
C40.0181 (7)0.0358 (8)0.0331 (8)0.0057 (6)0.0012 (6)0.0112 (6)
C50.0554 (10)0.0317 (8)0.0222 (7)0.0229 (7)0.0020 (7)0.0040 (6)
C60.0412 (9)0.0444 (9)0.0236 (7)0.0263 (7)0.0025 (6)0.0129 (7)
C70.0362 (9)0.0374 (9)0.0599 (12)0.0089 (7)0.0232 (8)0.0044 (8)
C80.0218 (7)0.0256 (7)0.0203 (7)0.0081 (6)0.0004 (5)0.0051 (5)
O30.0338 (6)0.0786 (9)0.0252 (6)0.0134 (6)0.0072 (5)0.0150 (6)
O40.0278 (6)0.0548 (7)0.0274 (6)0.0076 (5)0.0086 (5)0.0077 (5)
C100.0390 (11)0.0916 (17)0.0505 (12)0.0032 (10)0.0058 (9)0.0319 (12)
C90.0263 (7)0.0376 (8)0.0226 (7)0.0100 (6)0.0022 (6)0.0047 (6)
Geometric parameters (Å, º) top
Ni1—N12.1073 (12)C1—C21.517 (2)
Ni1—N32.1140 (12)C1—H1B0.9900
Ni1—N52.1192 (12)C1—H1A0.9900
Ni1—N22.1225 (12)C2—H2A0.9900
Ni1—N62.1274 (12)C2—H2B0.9900
Ni1—N42.1326 (12)C3—C41.516 (2)
O1—C81.2464 (17)C3—H3B0.9900
O2—C81.2378 (18)C3—H3A0.9900
N1—C11.4702 (19)C4—H4B0.9900
N1—H1NB0.876 (9)C4—H4A0.9900
N1—H1NA0.862 (9)C5—C61.513 (2)
N2—C21.4757 (19)C5—H5B0.9900
N2—H2NB0.867 (9)C5—H5A0.9900
N2—H2NA0.869 (9)C6—H6B0.9900
N3—C31.4718 (18)C6—H6A0.9900
N3—H3NB0.855 (9)C7—C81.512 (2)
N3—H3NA0.863 (9)C7—H7A0.9800
N4—C41.4739 (19)C7—H7B0.9800
N4—H4NB0.865 (9)C7—H7C0.9800
N4—H4NA0.865 (9)O3—C91.2389 (19)
N5—C51.474 (2)O4—C91.2518 (18)
N5—H5NB0.866 (9)C10—C91.515 (2)
N5—H5NA0.861 (9)C10—H10A0.9800
N6—C61.471 (2)C10—H10B0.9800
N6—H6NB0.869 (9)C10—H10C0.9800
N6—H6NA0.870 (9)
N1—Ni1—N3173.32 (5)C2—C1—H1B110.1
N1—Ni1—N591.41 (5)N1—C1—H1A110.1
N3—Ni1—N592.79 (5)C2—C1—H1A110.1
N1—Ni1—N282.37 (5)H1B—C1—H1A108.5
N3—Ni1—N294.05 (5)N2—C2—C1108.53 (12)
N5—Ni1—N2170.69 (5)N2—C2—H2A110.0
N1—Ni1—N696.03 (5)C1—C2—H2A110.0
N3—Ni1—N689.68 (5)N2—C2—H2B110.0
N5—Ni1—N682.34 (5)C1—C2—H2B110.0
N2—Ni1—N691.39 (5)H2A—C2—H2B108.4
N1—Ni1—N492.73 (5)N3—C3—C4108.78 (11)
N3—Ni1—N481.72 (5)N3—C3—H3B109.9
N5—Ni1—N495.22 (5)C4—C3—H3B109.9
N2—Ni1—N492.01 (5)N3—C3—H3A109.9
N6—Ni1—N4170.96 (5)C4—C3—H3A109.9
C1—N1—Ni1107.39 (9)H3B—C3—H3A108.3
C1—N1—H1NB107.0 (11)N4—C4—C3107.87 (11)
Ni1—N1—H1NB112.9 (11)N4—C4—H4B110.1
C1—N1—H1NA111.1 (11)C3—C4—H4B110.1
Ni1—N1—H1NA109.1 (11)N4—C4—H4A110.1
H1NB—N1—H1NA109.4 (16)C3—C4—H4A110.1
C2—N2—Ni1107.47 (9)H4B—C4—H4A108.4
C2—N2—H2NB111.9 (11)N5—C5—C6109.10 (12)
Ni1—N2—H2NB109.8 (11)N5—C5—H5B109.9
C2—N2—H2NA108.5 (11)C6—C5—H5B109.9
Ni1—N2—H2NA111.2 (11)N5—C5—H5A109.9
H2NB—N2—H2NA108.1 (16)C6—C5—H5A109.9
C3—N3—Ni1109.22 (8)H5B—C5—H5A108.3
C3—N3—H3NB107.8 (11)N6—C6—C5108.70 (12)
Ni1—N3—H3NB108.9 (11)N6—C6—H6B109.9
C3—N3—H3NA111.5 (11)C5—C6—H6B109.9
Ni1—N3—H3NA110.6 (11)N6—C6—H6A109.9
H3NB—N3—H3NA108.7 (15)C5—C6—H6A109.9
C4—N4—Ni1106.53 (8)H6B—C6—H6A108.3
C4—N4—H4NB110.3 (11)C8—C7—H7A109.5
Ni1—N4—H4NB118.1 (11)C8—C7—H7B109.5
C4—N4—H4NA107.5 (11)H7A—C7—H7B109.5
Ni1—N4—H4NA107.9 (11)C8—C7—H7C109.5
H4NB—N4—H4NA106.1 (16)H7A—C7—H7C109.5
C5—N5—Ni1106.97 (10)H7B—C7—H7C109.5
C5—N5—H5NB109.4 (12)O2—C8—O1124.58 (14)
Ni1—N5—H5NB111.8 (12)O2—C8—C7117.93 (13)
C5—N5—H5NA110.8 (12)O1—C8—C7117.44 (13)
Ni1—N5—H5NA108.9 (11)C9—C10—H10A109.5
H5NB—N5—H5NA108.9 (16)C9—C10—H10B109.5
C6—N6—Ni1108.00 (9)H10A—C10—H10B109.5
C6—N6—H6NB109.2 (12)C9—C10—H10C109.5
Ni1—N6—H6NB114.1 (12)H10A—C10—H10C109.5
C6—N6—H6NA109.5 (11)H10B—C10—H10C109.5
Ni1—N6—H6NA108.7 (12)O3—C9—O4125.16 (15)
H6NB—N6—H6NA107.3 (16)O3—C9—C10117.39 (15)
N1—C1—C2107.84 (12)O4—C9—C10117.45 (15)
N1—C1—H1B110.1
N3—Ni1—N1—C140.2 (4)N1—Ni1—N5—C579.04 (9)
N5—Ni1—N1—C1169.19 (10)N3—Ni1—N5—C5106.16 (9)
N2—Ni1—N1—C117.76 (10)N2—Ni1—N5—C531.2 (3)
N6—Ni1—N1—C1108.36 (10)N6—Ni1—N5—C516.85 (9)
N4—Ni1—N1—C173.90 (10)N4—Ni1—N5—C5171.91 (9)
N1—Ni1—N2—C212.57 (10)N1—Ni1—N6—C6103.11 (9)
N3—Ni1—N2—C2173.11 (10)N3—Ni1—N6—C680.37 (9)
N5—Ni1—N2—C235.9 (3)N5—Ni1—N6—C612.49 (9)
N6—Ni1—N2—C283.32 (10)N2—Ni1—N6—C6174.41 (9)
N4—Ni1—N2—C2105.06 (10)N4—Ni1—N6—C662.4 (3)
N1—Ni1—N3—C325.1 (4)Ni1—N1—C1—C244.48 (14)
N5—Ni1—N3—C3103.79 (9)Ni1—N2—C2—C140.20 (14)
N2—Ni1—N3—C382.52 (9)N1—C1—C2—N257.66 (17)
N6—Ni1—N3—C3173.89 (9)Ni1—N3—C3—C436.79 (13)
N4—Ni1—N3—C38.92 (9)Ni1—N4—C4—C346.53 (13)
N1—Ni1—N4—C4162.87 (9)N3—C3—C4—N456.57 (15)
N3—Ni1—N4—C420.87 (9)Ni1—N5—C5—C643.22 (14)
N5—Ni1—N4—C471.20 (9)Ni1—N6—C6—C539.26 (14)
N2—Ni1—N4—C4114.67 (9)N5—C5—C6—N656.38 (17)
N6—Ni1—N4—C42.7 (4)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1NA···O4i0.86 (1)2.29 (1)3.0370 (17)145 (1)
N1—H1NB···O40.88 (1)2.08 (1)2.9536 (17)172 (2)
N2—H2NA···O1ii0.87 (1)2.11 (1)2.9690 (18)170 (2)
N2—H2NB···O1iii0.87 (1)2.23 (1)3.0444 (17)157 (2)
N3—H3NA···O2iii0.86 (1)2.33 (1)3.1076 (17)150 (1)
N3—H3NB···O20.86 (1)2.09 (1)2.9316 (17)168 (2)
N4—H4NA···O1ii0.87 (1)2.25 (1)3.0762 (17)160 (2)
N4—H4NB···O3iv0.87 (1)2.21 (1)2.9916 (16)150 (2)
N5—H5NA···O4i0.86 (1)2.09 (1)2.9105 (17)158 (2)
N5—H5NB···O20.87 (1)2.44 (1)3.2254 (19)151 (2)
N6—H6NA···O2iii0.87 (1)2.48 (1)3.3102 (19)159 (2)
N6—H6NB···O30.87 (1)2.08 (1)2.9395 (18)171 (2)
Symmetry codes: (i) x+1, y+1, z+2; (ii) x, y+1, z; (iii) x+1, y+1, z+1; (iv) x+1, y, z.
Tris(ethylenediamine-κ2N,N')copper(II) diacetate (umd943_a) top
Crystal data top
[Cu(C2H8N2)3](C2H3O2)2Z = 2
Mr = 361.94F(000) = 386
Triclinic, P1Dx = 1.396 Mg m3
a = 8.2953 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 8.9144 (8) ÅCell parameters from 9890 reflections
c = 12.7148 (12) Åθ = 3.1–25.7°
α = 75.244 (4)°µ = 1.29 mm1
β = 85.082 (4)°T = 200 K
γ = 71.226 (4)°Block, blue
V = 860.84 (14) Å30.20 × 0.15 × 0.10 mm
Data collection top
Bruker CMOS
diffractometer
3287 independent reflections
Radiation source: fine-focus sealed tube2965 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.042
φ and ω scansθmax = 25.8°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2014)
h = 1010
Tmin = 0.782, Tmax = 0.882k = 1010
30526 measured reflectionsl = 1515
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)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.065H atoms treated by a mixture of independent and constrained refinement
S = 1.03 w = 1/[σ2(Fo2) + (0.0374P)2 + 0.3532P]
where P = (Fo2 + 2Fc2)/3
3287 reflections(Δ/σ)max = 0.001
228 parametersΔρmax = 0.51 e Å3
12 restraintsΔρmin = 0.28 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Cu10.56204 (2)0.64182 (2)0.718635 (15)0.02012 (8)
O10.6820 (2)0.0576 (2)0.58732 (16)0.0601 (5)
O20.74119 (19)0.28624 (16)0.52924 (12)0.0410 (3)
N10.51464 (19)0.68440 (18)0.87074 (12)0.0236 (3)
H1NB0.4303 (19)0.653 (2)0.9026 (15)0.028*
H1NA0.6045 (18)0.631 (2)0.9099 (14)0.028*
N20.4010 (2)0.9224 (2)0.67347 (14)0.0330 (4)
H2NB0.321 (2)0.947 (3)0.6269 (15)0.040*
H2NA0.467 (2)0.979 (2)0.6437 (17)0.040*
N30.61954 (19)0.61788 (19)0.56330 (12)0.0240 (3)
H3NB0.643 (3)0.5170 (13)0.5615 (17)0.029*
H3NA0.5324 (19)0.675 (2)0.5235 (14)0.029*
N40.7888 (2)0.6957 (2)0.70599 (13)0.0290 (3)
H4NB0.850 (2)0.667 (3)0.7638 (12)0.035*
H4NA0.763 (3)0.8004 (12)0.6837 (17)0.035*
N50.6611 (2)0.3534 (2)0.80270 (14)0.0360 (4)
H5NB0.727 (3)0.293 (2)0.7626 (16)0.043*
H5NA0.714 (3)0.339 (3)0.8623 (12)0.043*
N60.3432 (2)0.57903 (19)0.71268 (12)0.0266 (3)
H6NB0.264 (2)0.616 (2)0.7571 (14)0.032*
H6NA0.296 (3)0.625 (2)0.6498 (11)0.032*
C10.4703 (3)0.8600 (2)0.86476 (16)0.0336 (4)
H1B0.57280.89560.84610.040*
H1A0.42710.88170.93620.040*
C20.3349 (3)0.9538 (2)0.77858 (18)0.0358 (5)
H2A0.23190.91920.79780.043*
H2B0.30281.07220.77450.043*
C30.7694 (2)0.6710 (3)0.52449 (15)0.0326 (4)
H3B0.73370.79070.49450.039*
H3A0.82800.61760.46620.039*
C40.8881 (2)0.6244 (3)0.61917 (16)0.0339 (4)
H4B0.93320.50420.64480.041*
H4A0.98520.66750.59720.041*
C50.5004 (3)0.3162 (2)0.82757 (16)0.0352 (4)
H5B0.44830.35270.89340.042*
H5A0.52240.19680.84240.042*
C60.3794 (3)0.4017 (2)0.73268 (15)0.0323 (4)
H6B0.43100.36460.66690.039*
H6A0.27210.37400.74910.039*
C70.9451 (3)0.0645 (3)0.6394 (2)0.0439 (5)
H7A0.99480.14950.64180.066*
H7B1.02190.01160.59980.066*
H7C0.92870.00510.71370.066*
C80.7758 (2)0.1420 (2)0.58235 (14)0.0237 (4)
O30.04893 (19)0.6799 (2)0.85583 (12)0.0483 (4)
O40.22460 (17)0.61095 (18)0.99369 (11)0.0365 (3)
C100.0672 (3)0.7447 (4)1.0205 (2)0.0597 (7)
H10A0.17430.75110.98970.089*
H10B0.06880.85431.02250.089*
H10C0.05410.67481.09450.089*
C90.0803 (2)0.6732 (2)0.95066 (15)0.0296 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.01854 (12)0.02630 (12)0.01684 (12)0.00952 (8)0.00280 (7)0.00334 (8)
O10.0436 (9)0.0505 (10)0.0869 (14)0.0293 (8)0.0231 (9)0.0084 (9)
O20.0442 (9)0.0309 (7)0.0425 (8)0.0084 (6)0.0126 (7)0.0001 (6)
N10.0240 (8)0.0253 (7)0.0212 (8)0.0076 (6)0.0048 (6)0.0036 (6)
N20.0278 (9)0.0324 (9)0.0351 (9)0.0129 (7)0.0124 (7)0.0070 (7)
N30.0200 (7)0.0323 (8)0.0192 (7)0.0085 (6)0.0031 (6)0.0037 (6)
N40.0255 (8)0.0348 (8)0.0278 (8)0.0121 (7)0.0080 (6)0.0033 (7)
N50.0378 (10)0.0412 (10)0.0297 (9)0.0072 (8)0.0064 (7)0.0145 (7)
N60.0269 (8)0.0349 (8)0.0197 (7)0.0136 (7)0.0007 (6)0.0046 (6)
C10.0390 (11)0.0288 (10)0.0351 (11)0.0092 (8)0.0064 (8)0.0111 (8)
C20.0302 (10)0.0241 (9)0.0485 (12)0.0033 (8)0.0064 (9)0.0053 (8)
C30.0287 (10)0.0441 (11)0.0245 (9)0.0161 (8)0.0034 (8)0.0024 (8)
C40.0189 (9)0.0464 (11)0.0353 (11)0.0124 (8)0.0004 (8)0.0048 (9)
C50.0522 (13)0.0294 (10)0.0279 (10)0.0190 (9)0.0047 (9)0.0039 (8)
C60.0405 (11)0.0378 (10)0.0272 (10)0.0232 (9)0.0016 (8)0.0082 (8)
C70.0281 (11)0.0444 (12)0.0550 (14)0.0076 (9)0.0158 (10)0.0040 (10)
C80.0206 (9)0.0288 (9)0.0219 (9)0.0070 (7)0.0007 (7)0.0074 (7)
O30.0350 (8)0.0820 (12)0.0282 (8)0.0173 (8)0.0063 (6)0.0130 (7)
O40.0259 (7)0.0515 (8)0.0289 (7)0.0102 (6)0.0066 (6)0.0041 (6)
C100.0354 (13)0.087 (2)0.0552 (16)0.0080 (12)0.0065 (11)0.0303 (14)
C90.0246 (9)0.0386 (10)0.0260 (10)0.0118 (8)0.0010 (7)0.0060 (8)
Geometric parameters (Å, º) top
Cu1—N32.0400 (15)C1—C21.518 (3)
Cu1—N12.0461 (15)C1—H1B0.9900
Cu1—N42.0706 (16)C1—H1A0.9900
Cu1—N62.0765 (15)C2—H2A0.9900
Cu1—N22.3705 (16)C2—H2B0.9900
Cu1—N52.4123 (18)C3—C41.509 (3)
O1—C81.232 (2)C3—H3B0.9900
O2—C81.243 (2)C3—H3A0.9900
N1—C11.471 (2)C4—H4B0.9900
N1—H1NB0.867 (9)C4—H4A0.9900
N1—H1NA0.863 (9)C5—C61.514 (3)
N2—C21.460 (3)C5—H5B0.9900
N2—H2NB0.866 (10)C5—H5A0.9900
N2—H2NA0.862 (10)C6—H6B0.9900
N3—C31.472 (2)C6—H6A0.9900
N3—H3NB0.863 (9)C7—C81.507 (3)
N3—H3NA0.857 (9)C7—H7A0.9800
N4—C41.472 (3)C7—H7B0.9800
N4—H4NB0.865 (9)C7—H7C0.9800
N4—H4NA0.862 (9)O3—C91.238 (2)
N5—C51.464 (3)O4—C91.253 (2)
N5—H5NB0.865 (10)C10—C91.514 (3)
N5—H5NA0.869 (10)C10—H10A0.9800
N6—C61.469 (2)C10—H10B0.9800
N6—H6NB0.867 (9)C10—H10C0.9800
N6—H6NA0.863 (9)
N3—Cu1—N1174.30 (6)C2—C1—H1B109.9
N3—Cu1—N483.22 (6)N1—C1—H1A109.9
N1—Cu1—N492.17 (6)C2—C1—H1A109.9
N3—Cu1—N689.57 (6)H1B—C1—H1A108.3
N1—Cu1—N695.10 (6)N2—C2—C1109.31 (16)
N4—Cu1—N6172.68 (6)N2—C2—H2A109.8
N3—Cu1—N296.95 (6)C1—C2—H2A109.8
N1—Cu1—N279.80 (6)N2—C2—H2B109.8
N4—Cu1—N291.83 (6)C1—C2—H2B109.8
N6—Cu1—N290.25 (6)H2A—C2—H2B108.3
N3—Cu1—N595.62 (6)N3—C3—C4108.41 (15)
N1—Cu1—N588.48 (6)N3—C3—H3B110.0
N4—Cu1—N5100.32 (6)C4—C3—H3B110.0
N6—Cu1—N579.11 (6)N3—C3—H3A110.0
N2—Cu1—N5163.45 (6)C4—C3—H3A110.0
C1—N1—Cu1110.49 (11)H3B—C3—H3A108.4
C1—N1—H1NB106.9 (13)N4—C4—C3107.06 (15)
Cu1—N1—H1NB112.4 (14)N4—C4—H4B110.3
C1—N1—H1NA110.4 (13)C3—C4—H4B110.3
Cu1—N1—H1NA108.4 (14)N4—C4—H4A110.3
H1NB—N1—H1NA108.2 (19)C3—C4—H4A110.3
C2—N2—Cu1103.17 (11)H4B—C4—H4A108.6
C2—N2—H2NB112.3 (15)N5—C5—C6110.01 (16)
Cu1—N2—H2NB114.1 (15)N5—C5—H5B109.7
C2—N2—H2NA112.5 (16)C6—C5—H5B109.7
Cu1—N2—H2NA109.0 (16)N5—C5—H5A109.7
H2NB—N2—H2NA106 (2)C6—C5—H5A109.7
C3—N3—Cu1109.69 (11)H5B—C5—H5A108.2
C3—N3—H3NB108.5 (14)N6—C6—C5109.59 (15)
Cu1—N3—H3NB109.9 (14)N6—C6—H6B109.8
C3—N3—H3NA111.4 (14)C5—C6—H6B109.8
Cu1—N3—H3NA108.2 (14)N6—C6—H6A109.8
H3NB—N3—H3NA109.2 (19)C5—C6—H6A109.8
C4—N4—Cu1106.50 (11)H6B—C6—H6A108.2
C4—N4—H4NB110.4 (15)C8—C7—H7A109.5
Cu1—N4—H4NB118.4 (15)C8—C7—H7B109.5
C4—N4—H4NA107.6 (15)H7A—C7—H7B109.5
Cu1—N4—H4NA106.3 (15)C8—C7—H7C109.5
H4NB—N4—H4NA107 (2)H7A—C7—H7C109.5
C5—N5—Cu1101.64 (12)H7B—C7—H7C109.5
C5—N5—H5NB111.5 (16)O1—C8—O2123.50 (17)
Cu1—N5—H5NB115.3 (16)O1—C8—C7118.44 (17)
C5—N5—H5NA110.4 (16)O2—C8—C7117.99 (16)
Cu1—N5—H5NA108.4 (15)C9—C10—H10A109.5
H5NB—N5—H5NA109 (2)C9—C10—H10B109.5
C6—N6—Cu1112.03 (12)H10A—C10—H10B109.5
C6—N6—H6NB109.2 (14)C9—C10—H10C109.5
Cu1—N6—H6NB113.4 (14)H10A—C10—H10C109.5
C6—N6—H6NA109.0 (14)H10B—C10—H10C109.5
Cu1—N6—H6NA109.7 (14)O3—C9—O4125.11 (18)
H6NB—N6—H6NA103 (2)O3—C9—C10117.52 (19)
N1—C1—C2109.09 (15)O4—C9—C10117.37 (18)
N1—C1—H1B109.9
N3—Cu1—N1—C135.2 (6)N3—Cu1—N5—C5103.95 (12)
N4—Cu1—N1—C171.09 (13)N1—Cu1—N5—C580.02 (12)
N6—Cu1—N1—C1109.71 (12)N4—Cu1—N5—C5171.95 (11)
N2—Cu1—N1—C120.38 (12)N6—Cu1—N5—C515.47 (11)
N5—Cu1—N1—C1171.37 (13)N2—Cu1—N5—C535.3 (3)
N3—Cu1—N2—C2174.23 (11)N3—Cu1—N6—C680.73 (12)
N1—Cu1—N2—C210.51 (11)N1—Cu1—N6—C6102.54 (12)
N4—Cu1—N2—C2102.38 (12)N4—Cu1—N6—C671.1 (5)
N6—Cu1—N2—C284.63 (12)N2—Cu1—N6—C6177.68 (12)
N5—Cu1—N2—C235.1 (3)N5—Cu1—N6—C615.07 (12)
N1—Cu1—N3—C328.8 (7)Cu1—N1—C1—C249.05 (19)
N4—Cu1—N3—C37.34 (12)Cu1—N2—C2—C138.40 (16)
N6—Cu1—N3—C3173.89 (12)N1—C1—C2—N260.3 (2)
N2—Cu1—N3—C383.69 (12)Cu1—N3—C3—C435.02 (18)
N5—Cu1—N3—C3107.10 (12)Cu1—N4—C4—C346.65 (17)
N3—Cu1—N4—C422.06 (12)N3—C3—C4—N454.8 (2)
N1—Cu1—N4—C4161.30 (12)Cu1—N5—C5—C642.63 (17)
N6—Cu1—N4—C412.4 (5)Cu1—N6—C6—C544.14 (19)
N2—Cu1—N4—C4118.84 (12)N5—C5—C6—N660.8 (2)
N5—Cu1—N4—C472.45 (12)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1NB···O40.87 (1)2.06 (1)2.917 (2)170 (2)
N1—H1NA···O4i0.86 (1)2.27 (1)3.040 (2)149 (2)
N2—H2NB···O1ii0.87 (1)2.74 (2)3.393 (3)134 (2)
N2—H2NA···O1iii0.86 (1)2.12 (1)2.964 (2)165 (2)
N3—H3NB···O20.86 (1)2.09 (1)2.933 (2)167 (2)
N3—H3NA···O2ii0.86 (1)2.32 (1)3.085 (2)150 (2)
N4—H4NB···O3iv0.87 (1)2.15 (1)2.945 (2)153 (2)
N4—H4NA···O1iii0.86 (1)2.22 (1)3.062 (2)165 (2)
N5—H5NB···O20.87 (1)2.98 (2)3.647 (2)136 (2)
N5—H5NA···O4i0.87 (1)2.13 (1)2.956 (2)159 (2)
N6—H6NB···O30.87 (1)2.10 (1)2.956 (2)169 (2)
N6—H6NA···O2ii0.86 (1)2.22 (1)3.056 (2)162 (2)
Symmetry codes: (i) x+1, y+1, z+2; (ii) x+1, y+1, z+1; (iii) x, y+1, z; (iv) x+1, y, z.
Tris(ethylenediamine-κ2N,N')zinc(II) diacetate (umd886) top
Crystal data top
[Zn(C2H8N2)3](C2H3O2)2Z = 2
Mr = 363.77F(000) = 388
Triclinic, P1Dx = 1.368 Mg m3
a = 8.3223 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.1059 (5) ÅCell parameters from 9943 reflections
c = 12.7492 (7) Åθ = 3.1–26.0°
α = 70.855 (2)°µ = 1.41 mm1
β = 85.800 (2)°T = 200 K
γ = 75.434 (2)°Block, colourless
V = 883.34 (9) Å30.50 × 0.40 × 0.40 mm
Data collection top
Bruker CMOS
diffractometer
3450 independent reflections
Radiation source: fine-focus sealed tube3242 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
φ and ω scansθmax = 26.1°, θmin = 3.1°
Absorption correction: multi-scan
(SADABS; Bruker, 2014)
h = 1010
Tmin = 0.538, Tmax = 0.602k = 1111
14208 measured reflectionsl = 1515
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)] = 0.020H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.051 w = 1/[σ2(Fo2) + (0.0238P)2 + 0.3152P]
where P = (Fo2 + 2Fc2)/3
S = 1.08(Δ/σ)max = 0.026
3450 reflectionsΔρmax = 0.30 e Å3
229 parametersΔρmin = 0.24 e Å3
12 restraintsExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.028 (2)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Zn10.564211 (18)0.644619 (18)0.713369 (12)0.01994 (8)
O10.73399 (15)0.04251 (14)0.55873 (10)0.0401 (3)
O20.71151 (18)0.27798 (15)0.57743 (14)0.0605 (4)
N10.52981 (16)0.68995 (15)0.87028 (10)0.0259 (3)
H1NB0.4439 (16)0.659 (2)0.9049 (13)0.031*
H1NA0.6163 (16)0.6385 (18)0.9120 (12)0.031*
N20.44734 (15)0.90194 (14)0.65359 (10)0.0258 (3)
H2NB0.3715 (17)0.922 (2)0.6044 (12)0.031*
H2NA0.5207 (18)0.9544 (19)0.6234 (13)0.031*
N30.62038 (14)0.62314 (14)0.54859 (9)0.0220 (2)
H3NB0.636 (2)0.5237 (12)0.5542 (14)0.026*
H3NA0.5383 (16)0.6788 (17)0.5037 (12)0.026*
N40.81600 (15)0.68484 (15)0.69240 (10)0.0260 (3)
H4NB0.8797 (19)0.651 (2)0.7505 (11)0.031*
H4NA0.807 (2)0.7873 (11)0.6653 (14)0.031*
N50.63463 (17)0.38640 (15)0.79660 (11)0.0301 (3)
H5NB0.689 (2)0.339 (2)0.7518 (13)0.036*
H5NA0.6965 (19)0.366 (2)0.8537 (11)0.036*
N60.32494 (16)0.58718 (17)0.70605 (11)0.0306 (3)
H6NB0.2521 (18)0.623 (2)0.7499 (13)0.037*
H6NA0.285 (2)0.634 (2)0.6392 (9)0.037*
C10.5017 (2)0.86365 (18)0.84717 (13)0.0338 (3)
H1B0.60770.89630.82780.041*
H1A0.45660.89260.91370.041*
C20.3789 (2)0.94863 (19)0.75082 (13)0.0341 (3)
H2A0.27170.91870.77140.041*
H2B0.35901.06610.73300.041*
C30.77475 (17)0.67284 (18)0.50930 (12)0.0267 (3)
H3B0.75070.79090.47670.032*
H3A0.82440.62580.45110.032*
C40.89558 (17)0.61677 (19)0.60607 (13)0.0295 (3)
H4B0.92470.49830.63620.035*
H4A0.99870.65290.58100.035*
C50.4799 (2)0.3337 (2)0.83065 (13)0.0369 (4)
H5B0.43470.36340.89690.044*
H5A0.50280.21580.85020.044*
C60.3544 (2)0.4127 (2)0.73609 (13)0.0352 (4)
H6B0.39710.37840.67110.042*
H6A0.24910.38000.75910.042*
C70.9469 (2)0.0720 (2)0.65678 (17)0.0451 (4)
H7A0.97730.15870.67420.068*
H7B1.03370.02820.61150.068*
H7C0.93520.01270.72590.068*
C80.78433 (17)0.13645 (16)0.59340 (11)0.0235 (3)
O30.06083 (15)0.67616 (17)0.85582 (10)0.0469 (3)
O40.23264 (13)0.61786 (15)0.99611 (9)0.0386 (3)
C100.0498 (2)0.7418 (3)1.01481 (18)0.0599 (6)
H10A0.15290.77580.97160.090*
H10B0.02750.83411.02930.090*
H10C0.06100.65971.08550.090*
C90.09244 (18)0.67346 (19)0.95009 (12)0.0297 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn10.02054 (10)0.02266 (10)0.01683 (10)0.00357 (6)0.00355 (6)0.00704 (6)
O10.0490 (7)0.0347 (6)0.0405 (7)0.0163 (5)0.0155 (5)0.0092 (5)
O20.0593 (9)0.0359 (7)0.0863 (11)0.0160 (6)0.0384 (8)0.0318 (7)
N10.0280 (6)0.0290 (6)0.0193 (6)0.0026 (5)0.0054 (5)0.0080 (5)
N20.0267 (6)0.0257 (6)0.0227 (6)0.0025 (5)0.0073 (5)0.0063 (5)
N30.0206 (6)0.0263 (6)0.0202 (6)0.0037 (5)0.0036 (4)0.0095 (5)
N40.0230 (6)0.0300 (6)0.0264 (6)0.0059 (5)0.0079 (5)0.0093 (5)
N50.0404 (7)0.0270 (6)0.0225 (6)0.0052 (5)0.0090 (5)0.0077 (5)
N60.0267 (6)0.0447 (8)0.0230 (6)0.0129 (6)0.0020 (5)0.0106 (6)
C10.0459 (9)0.0322 (8)0.0262 (8)0.0046 (7)0.0068 (7)0.0154 (6)
C20.0397 (9)0.0275 (8)0.0316 (8)0.0037 (6)0.0062 (7)0.0124 (6)
C30.0249 (7)0.0330 (8)0.0230 (7)0.0069 (6)0.0022 (5)0.0108 (6)
C40.0184 (7)0.0365 (8)0.0333 (8)0.0033 (6)0.0016 (6)0.0129 (7)
C50.0593 (11)0.0338 (8)0.0223 (7)0.0242 (8)0.0018 (7)0.0052 (6)
C60.0433 (9)0.0477 (9)0.0259 (7)0.0267 (8)0.0033 (7)0.0157 (7)
C70.0340 (9)0.0367 (9)0.0607 (12)0.0091 (7)0.0215 (8)0.0054 (8)
C80.0217 (7)0.0256 (7)0.0228 (7)0.0070 (5)0.0010 (5)0.0060 (6)
O30.0355 (6)0.0786 (9)0.0280 (6)0.0117 (6)0.0080 (5)0.0186 (6)
O40.0277 (6)0.0560 (7)0.0282 (6)0.0060 (5)0.0085 (4)0.0096 (5)
C100.0402 (11)0.0850 (16)0.0530 (12)0.0019 (10)0.0051 (9)0.0309 (12)
C90.0269 (7)0.0364 (8)0.0232 (7)0.0085 (6)0.0027 (6)0.0048 (6)
Geometric parameters (Å, º) top
Zn1—N12.1570 (12)C1—C21.521 (2)
Zn1—N32.1795 (11)C1—H1B0.9900
Zn1—N52.1816 (13)C1—H1A0.9900
Zn1—N22.1927 (12)C2—H2A0.9900
Zn1—N62.1979 (13)C2—H2B0.9900
Zn1—N42.1992 (12)C3—C41.518 (2)
O1—C81.2482 (17)C3—H3B0.9900
O2—C81.2340 (18)C3—H3A0.9900
N1—C11.4702 (19)C4—H4B0.9900
N1—H1NB0.873 (9)C4—H4A0.9900
N1—H1NA0.862 (9)C5—C61.516 (2)
N2—C21.4705 (19)C5—H5B0.9900
N2—H2NB0.865 (9)C5—H5A0.9900
N2—H2NA0.861 (9)C6—H6B0.9900
N3—C31.4683 (18)C6—H6A0.9900
N3—H3NB0.861 (9)C7—C81.509 (2)
N3—H3NA0.862 (9)C7—H7A0.9800
N4—C41.4725 (19)C7—H7B0.9800
N4—H4NB0.867 (9)C7—H7C0.9800
N4—H4NA0.867 (9)O3—C91.2402 (19)
N5—C51.473 (2)O4—C91.2531 (18)
N5—H5NB0.864 (9)C10—C91.514 (2)
N5—H5NA0.864 (9)C10—H10A0.9800
N6—C61.466 (2)C10—H10B0.9800
N6—H6NB0.868 (9)C10—H10C0.9800
N6—H6NA0.867 (9)
N1—Zn1—N3171.96 (5)C2—C1—H1B110.0
N1—Zn1—N591.47 (5)N1—C1—H1A110.0
N3—Zn1—N593.65 (5)C2—C1—H1A110.0
N1—Zn1—N280.77 (5)H1B—C1—H1A108.4
N3—Zn1—N295.17 (5)N2—C2—C1109.05 (12)
N5—Zn1—N2167.64 (5)N2—C2—H2A109.9
N1—Zn1—N697.84 (5)C1—C2—H2A109.9
N3—Zn1—N689.12 (5)N2—C2—H2B109.9
N5—Zn1—N680.45 (5)C1—C2—H2B109.9
N2—Zn1—N691.02 (5)H2A—C2—H2B108.3
N1—Zn1—N493.33 (5)N3—C3—C4109.35 (11)
N3—Zn1—N479.87 (4)N3—C3—H3B109.8
N5—Zn1—N497.39 (5)C4—C3—H3B109.8
N2—Zn1—N492.68 (5)N3—C3—H3A109.8
N6—Zn1—N4168.66 (5)C4—C3—H3A109.8
C1—N1—Zn1107.66 (9)H3B—C3—H3A108.3
C1—N1—H1NB109.0 (11)N4—C4—C3108.38 (11)
Zn1—N1—H1NB111.0 (12)N4—C4—H4B110.0
C1—N1—H1NA111.1 (11)C3—C4—H4B110.0
Zn1—N1—H1NA109.8 (11)N4—C4—H4A110.0
H1NB—N1—H1NA108.2 (16)C3—C4—H4A110.0
C2—N2—Zn1107.24 (9)H4B—C4—H4A108.4
C2—N2—H2NB112.0 (11)N5—C5—C6109.39 (12)
Zn1—N2—H2NB110.4 (11)N5—C5—H5B109.8
C2—N2—H2NA109.1 (12)C6—C5—H5B109.8
Zn1—N2—H2NA109.8 (12)N5—C5—H5A109.8
H2NB—N2—H2NA108.4 (17)C6—C5—H5A109.8
C3—N3—Zn1109.34 (8)H5B—C5—H5A108.2
C3—N3—H3NB108.2 (11)N6—C6—C5109.23 (12)
Zn1—N3—H3NB107.9 (11)N6—C6—H6B109.8
C3—N3—H3NA111.9 (11)C5—C6—H6B109.8
Zn1—N3—H3NA110.2 (11)N6—C6—H6A109.8
H3NB—N3—H3NA109.2 (15)C5—C6—H6A109.8
C4—N4—Zn1106.68 (8)H6B—C6—H6A108.3
C4—N4—H4NB110.9 (12)C8—C7—H7A109.5
Zn1—N4—H4NB118.4 (12)C8—C7—H7B109.5
C4—N4—H4NA106.3 (12)H7A—C7—H7B109.5
Zn1—N4—H4NA107.7 (12)C8—C7—H7C109.5
H4NB—N4—H4NA106.2 (16)H7A—C7—H7C109.5
C5—N5—Zn1107.04 (10)H7B—C7—H7C109.5
C5—N5—H5NB110.3 (12)O2—C8—O1124.29 (14)
Zn1—N5—H5NB110.1 (12)O2—C8—C7118.48 (13)
C5—N5—H5NA110.7 (12)O1—C8—C7117.22 (13)
Zn1—N5—H5NA109.6 (12)C9—C10—H10A109.5
H5NB—N5—H5NA109.1 (17)C9—C10—H10B109.5
C6—N6—Zn1107.98 (10)H10A—C10—H10B109.5
C6—N6—H6NB110.3 (12)C9—C10—H10C109.5
Zn1—N6—H6NB112.2 (12)H10A—C10—H10C109.5
C6—N6—H6NA110.6 (12)H10B—C10—H10C109.5
Zn1—N6—H6NA109.0 (12)O3—C9—O4125.10 (15)
H6NB—N6—H6NA106.7 (17)O3—C9—C10117.38 (15)
N1—C1—C2108.35 (12)O4—C9—C10117.51 (15)
N1—C1—H1B110.0
N3—Zn1—N1—C142.4 (4)N1—Zn1—N5—C580.33 (9)
N5—Zn1—N1—C1171.99 (10)N3—Zn1—N5—C5105.87 (9)
N2—Zn1—N1—C117.69 (10)N2—Zn1—N5—C529.6 (3)
N6—Zn1—N1—C1107.45 (10)N6—Zn1—N5—C517.38 (9)
N4—Zn1—N1—C174.50 (10)N4—Zn1—N5—C5173.88 (9)
N1—Zn1—N2—C212.85 (10)N1—Zn1—N6—C6102.59 (9)
N3—Zn1—N2—C2174.15 (10)N3—Zn1—N6—C681.44 (9)
N5—Zn1—N2—C238.8 (3)N5—Zn1—N6—C612.41 (9)
N6—Zn1—N2—C284.93 (10)N2—Zn1—N6—C6176.59 (9)
N4—Zn1—N2—C2105.79 (10)N4—Zn1—N6—C667.5 (3)
N1—Zn1—N3—C323.2 (4)Zn1—N1—C1—C244.88 (14)
N5—Zn1—N3—C3106.29 (9)Zn1—N2—C2—C140.74 (15)
N2—Zn1—N3—C382.39 (9)N1—C1—C2—N258.83 (17)
N6—Zn1—N3—C3173.34 (9)Zn1—N3—C3—C437.57 (13)
N4—Zn1—N3—C39.43 (9)Zn1—N4—C4—C346.77 (13)
N1—Zn1—N4—C4163.77 (9)N3—C3—C4—N457.74 (15)
N3—Zn1—N4—C420.56 (9)Zn1—N5—C5—C644.32 (14)
N5—Zn1—N4—C471.85 (10)Zn1—N6—C6—C539.81 (14)
N2—Zn1—N4—C4115.33 (9)N5—C5—C6—N658.02 (17)
N6—Zn1—N4—C46.4 (3)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1NB···O40.87 (1)2.08 (1)2.9437 (17)170 (2)
N1—H1NA···O4i0.86 (1)2.31 (1)3.0398 (17)142 (2)
N2—H2NB···O1ii0.87 (1)2.21 (1)3.0293 (16)158 (2)
N2—H2NA···O1iii0.86 (1)2.13 (1)2.9816 (18)170 (2)
N3—H3NB···O20.86 (1)2.09 (1)2.9449 (17)171 (2)
N3—H3NA···O2ii0.86 (1)2.28 (1)3.0775 (17)155 (2)
N4—H4NB···O3iv0.87 (1)2.19 (1)2.9885 (16)153 (2)
N4—H4NA···O1iii0.87 (1)2.23 (1)3.0642 (17)163 (2)
N5—H5NB···O20.86 (1)2.44 (1)3.228 (2)151 (2)
N5—H5NA···O4i0.86 (1)2.11 (1)2.9232 (16)158 (2)
N6—H6NB···O30.87 (1)2.08 (1)2.9390 (18)171 (2)
N6—H6NA···O2ii0.87 (1)2.61 (1)3.424 (2)157 (2)
Symmetry codes: (i) x+1, y+1, z+2; (ii) x+1, y+1, z+1; (iii) x, y+1, z; (iv) x+1, y, z.
Selected bond lengths (Å) for the [M(en)3](OAc)2 series top
MnFeCoNiCuZn
M1—N12.2459 (12)2.1880 (17)2.1455 (14)2.1073 (12)2.0461 (15)2.1570 (12)
M1—N22.2740 (13)2.2147 (18)2.1735 (14)2.1225 (12)2.3705 (16)2.1927 (12)
M1—N32.2680 (12)2.2062 (16)2.1625 (13)2.1140 (12)2.0400 (15)2.1795 (11)
M1—N42.2797 (13)2.2183 (18)2.1757 (14)2.1326 (12)2.0706 (16)2.1992 (12)
M1—N52.2699 (13)2.2115 (19)2.1708 (15)2.1192 (12)2.4123 (18)2.1816 (13)
M1—N62.2784 (13)2.2124 (18)2.1687 (15)2.1274 (12)2.0765 (15)2.1979 (13)
M—N (average)2.26932.20852.16612.12052.16932.1847
 

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