research papers
A new [Ni(NH2CH2CH2NH2)2](V6O14) compound has been synthesized hydrothermally and was found to crystallize in the monoclinic system. The single-crystal X-ray data leads to a disordered structure, which can be decomposed into two ordered models with different stacking of the V6O14 layers. The structure of the layer is the same in both models and represents a new member of the V6O14 series. All known structures from this series are constructed from the same chain of square pyramids (SP), which share alternatively adjacent or opposite edges of their bases. The differences lie in the orientation of the SP chains which are joined together by sharing corners with tetrahedra to form the layers. Combinatorial analysis of the V6O14 structures was conducted, yielding ten possible symmetry groups for the series of V6O14 layers. The known structures belong only to the three simplest cases with the highest symmetry.
Supporting information
CCDC references: 138549; 138550
Computing details top
Data collection: SMART (Siemens, 1995) for OD-en2NiV6O14. Cell refinement: SAINT (Siemens, 1995) for OD-en2NiV6O14. Data reduction: SAINT for OD-en2NiV6O14. Program(s) used to solve structure: CSD (Akeslrud et al., 1993) for OD-en2NiV6O14. Program(s) used to refine structure: CSD for OD-en2NiV6O14. Molecular graphics: ORTEPIII (Farrugia, 1997), CrystalDesigner (1997) for OD-en2NiV6O14. Software used to prepare material for publication: CSD for OD-en2NiV6O14.
(OD-en2NiV6O14) bis-ethylenediamine nickel hexavanadium tetradecaoxide top
Crystal data top
(NH2CH2CH2NH2)2NiV6O14 | F(000) = 692 |
Mr = 708.59 | Dx = 2.497 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 8.9311 (11) Å | Cell parameters from 1430 reflections |
b = 17.127 (2) Å | θ = 4.7–28° |
c = 6.6270 (8) Å | µ = 3.90 mm−1 |
β = 111.610 (2)° | T = 295 K |
V = 942.4 (3) Å3 | Plate, black |
Z = 2 | 0.41 × 0.16 × 0.06 mm |
Data collection top
Siemens Smart CCD diffractometer | 1684 independent reflections |
Radiation source: sealed tube | 1267 reflections with Fo > 4σ(Fo) |
Graphite monochromator | Rint = 0.051 |
ω scans | θmax = 28°, θmin = 3.1° |
Absorption correction: multi-scan SADABS (sheldrick, 1996) | h = −8→2 |
Tmin = 0.641, Tmax = 0.777 | k = −11→4 |
3679 measured reflections | l = −21→20 |
Refinement top
Refinement on F | H-atom parameters not refined |
Least-squares matrix: full with fixed elements per cycle | w = 1/[σ(Fo)2 + 0.002Fo2)] |
R[F2 > 2σ(F2)] = 0.060 | (Δ/σ)max = 0.01 |
wR(F2) = 0.0637 | Δρmax = 0.93 e Å−3 |
1267 reflections | Δρmin = 1.22 e Å−3 |
165 parameters |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | Occ. (<1) | |
V1 | 0.50362 (1) | 0.20999 (7) | 0.1424 (2) | 0.0079 (5) | |
V2 | 0.2310 (3) | 0.2133 (2) | 0.2810 (5) | 0.0099 (4) | 0.5 |
V3 | 0.7774 (3) | 0.2894 (2) | 0.0584 (5) | 0.0107 (4) | 0.5 |
V4 | 0.1761 (3) | 0.2878 (2) | 0.7532 (5) | 0.0099 (4) | 0.5 |
V5 | 0.8294 (3) | 0.2133 (2) | 0.5882 (5) | 0.0107 (4) | 0.5 |
O1 | 0.5012 (6) | 0.1194 (3) | 0.0690 (8) | 0.017 (2) | |
O2 | 0.1915 (7) | 0.1213 (3) | 0.2816 (9) | 0.023 (2) | |
O3 | 0.8104 (7) | 0.3796 (3) | 0.1123 (9) | 0.025 (2) | |
O4 | 0.277 (2) | 0.2578 (8) | 0.574 (2) | 0.013 (2) | 0.5 |
O5 | 0.735 (2) | 0.2399 (8) | 0.303 (2) | 0.017 (2) | 0.5 |
O6 | 0.4683 (14) | 0.2191 (7) | 0.404 (2) | 0.016 (2) | 0.5 |
O7 | −0.0196 (14) | 0.2669 (7) | 0.644 (2) | 0.019 (2) | 0.5 |
O8 | 0.269 (2) | 0.2373 (8) | 0.018 (2) | 0.013 (2) | 0.5 |
O9 | 0.736 (2) | 0.2686 (8) | 0.752 (2) | 0.017 (2) | 0.5 |
O10 | 0.5417 (14) | 0.2807 (7) | −0.055 (2) | 0.016 (2) | 0.5 |
O11 | 1.0262 (14) | 0.2304 (7) | 0.671 (2) | 0.019 (2) | 0.5 |
Ni | 0.5 | 0.5 | 0.5 | 0.0125 (6) | |
C1 | 0.1524 (10) | 0.5164 (6) | 0.3504 (14) | 0.028 (4) | |
C2 | 0.1855 (11) | 0.4566 (6) | 0.201 (2) | 0.033 (4) | |
N1 | 0.2871 (9) | 0.5160 (4) | 0.5629 (11) | 0.025 (3) | |
N2 | 0.3419 (8) | 0.4757 (4) | 0.1903 (10) | 0.021 (3) | |
H1 | 0.05398 | 0.50396 | 0.36866 | 0.05066* | |
H2 | 0.14310 | 0.56683 | 0.28603 | 0.05066* | |
H3 | 0.10262 | 0.45748 | 0.05737 | 0.05066* | |
H4 | 0.18760 | 0.40419 | 0.25675 | 0.05066* | |
H5 | 0.27280 | 0.47393 | 0.64993 | 0.05066* | |
H6 | 0.28996 | 0.56364 | 0.63726 | 0.05066* | |
H7 | 0.33109 | 0.52004 | 0.09848 | 0.05066* | |
H8 | 0.38157 | 0.43301 | 0.13069 | 0.05066* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
V1 | 0.0041 (7) | 0.0121 (7) | 0.0077 (7) | 0.0000 (5) | 0.0023 (7) | −0.0002 (5) |
O1 | 0.016 (3) | 0.018 (3) | 0.015 (3) | −0.004 (2) | 0.004 (3) | −0.007 (2) |
O2 | 0.027 (4) | 0.016 (3) | 0.027 (4) | −0.005 (3) | 0.012 (3) | −0.001 (3) |
O3 | 0.033 (4) | 0.017 (3) | 0.028 (3) | −0.005 (3) | 0.014 (3) | −0.005 (3) |
Ni | 0.0115 (8) | 0.0142 (8) | 0.0116 (8) | −0.0012 (6) | 0.0041 (7) | 0.0011 (6) |
C1 | 0.006 (5) | 0.045 (7) | 0.026 (6) | 0.004 (4) | −0.001 (5) | 0.007 (5) |
C2 | 0.008 (5) | 0.050 (7) | 0.025 (6) | −0.003 (5) | −0.012 (5) | 0.000 (5) |
N1 | 0.030 (4) | 0.024 (4) | 0.031 (4) | −0.004 (3) | 0.022 (4) | 0.001 (3) |
N2 | 0.018 (4) | 0.028 (4) | 0.016 (4) | 0.002 (3) | 0.003 (4) | −0.001 (3) |
Geometric parameters (Å, º) top
V1—O1 | 1.624 (6) | V5—O7vii | 1.559 (13) |
V1—O6 | 1.876 (12) | V5—O3i | 1.614 (7) |
V1—O10 | 1.900 (12) | V5—O11 | 1.663 (14) |
V1—O10i | 1.916 (12) | V5—O5 | 1.823 (13) |
V1—O6ii | 1.927 (12) | V5—O9 | 1.853 (15) |
V1—O9ii | 1.97 (2) | V5—O10i | 2.392 (13) |
V1—O4ii | 1.98 (2) | O1—Niviii | 2.095 (5) |
V1—O8 | 2.01 (2) | O6—O10i | 0.61 (2) |
V2—O2 | 1.617 (6) | O7—O11v | 0.73 (2) |
V2—O4ii | 1.646 (14) | Ni—N2 | 2.060 (6) |
V2—O8i | 1.707 (13) | Ni—N2ix | 2.060 (6) |
V2—O11iii | 1.955 (13) | Ni—N1 | 2.109 (8) |
V2—O6 | 1.973 (13) | Ni—N1ix | 2.109 (8) |
V3—O3 | 1.590 (7) | C1—H2 | 0.953 |
V3—O5ii | 1.673 (13) | C1—H1 | 0.954 |
V3—O9ii | 1.765 (15) | C1—N1 | 1.477 (12) |
V3—O7iv | 1.944 (13) | C1—C2 | 1.527 (14) |
V3—O10 | 1.963 (13) | C2—H3 | 0.967 |
V4—O2i | 1.569 (6) | C2—H4 | 0.969 |
V4—O11v | 1.586 (13) | C2—N2 | 1.461 (13) |
V4—O7 | 1.666 (13) | N1—H6 | 0.949 |
V4—O4 | 1.809 (15) | N1—H5 | 0.960 |
V4—O8vi | 1.857 (13) | N2—H7 | 0.956 |
V4—O6i | 2.430 (13) | N2—H8 | 0.958 |
O1—V1—O6 | 111.6 (4) | O5—V5—O9 | 110.2 (7) |
O1—V1—O10 | 112.9 (4) | O5—V5—O10i | 64.0 (6) |
O1—V1—O10i | 111.8 (4) | O9—V5—O10i | 63.9 (6) |
O1—V1—O6ii | 112.1 (4) | V1—O1—Niviii | 175.3 (3) |
O1—V1—O9ii | 100.6 (5) | V4ii—O2—V2 | 16.4 (2) |
O1—V1—O4ii | 107.3 (5) | V3—O3—V5ii | 15.6 (2) |
O1—V1—O8 | 101.7 (5) | V2i—O4—V2 | 155.1 (9) |
O6—V1—O10 | 135.5 (5) | V2i—O4—V1i | 105.8 (7) |
O6—V1—O10i | 18.5 (5) | V2—O4—V1i | 99.0 (6) |
O6—V1—O6ii | 132.3 (5) | V3i—O5—V3 | 156.4 (9) |
O6—V1—O9ii | 99.1 (6) | V3i—O5—V1 | 105.2 (7) |
O6—V1—O4ii | 71.6 (6) | V3—O5—V1 | 98.4 (6) |
O6—V1—O8 | 81.5 (6) | O10i—O6—V1 | 84.5 (16) |
O10—V1—O10i | 131.2 (5) | O10i—O6—V1i | 78.4 (16) |
O10—V1—O6ii | 18.3 (5) | O10i—O6—V2 | 176.4 (19) |
O10—V1—O9ii | 72.7 (6) | V1—O6—V1i | 141.1 (7) |
O10—V1—O4ii | 95.2 (6) | V1—O6—V2 | 97.8 (6) |
O10—V1—O8 | 89.7 (6) | V1i—O6—V2 | 101.3 (6) |
O10i—V1—O6ii | 136.1 (5) | O11v—O7—V5v | 85.0 (14) |
O10i—V1—O9ii | 80.9 (6) | O11v—O7—V4 | 71.0 (14) |
O10i—V1—O4ii | 89.3 (6) | V5v—O7—V4 | 155.1 (9) |
O10i—V1—O8 | 99.5 (6) | V2ii—O8—V2 | 153.4 (9) |
O6ii—V1—O9ii | 91.0 (6) | V2ii—O8—V1 | 108.3 (7) |
O6ii—V1—O4ii | 78.0 (6) | V2—O8—V1 | 94.8 (6) |
O6ii—V1—O8 | 71.7 (6) | V3i—O9—V3vi | 147.8 (9) |
O9ii—V1—O4ii | 152.0 (6) | V3i—O9—V1i | 108.2 (7) |
O9ii—V1—O8 | 155.6 (6) | V3vi—O9—V1i | 96.8 (7) |
O4ii—V1—O8 | 10.3 (6) | O6ii—O10—V1 | 83.3 (16) |
O2—V2—O4ii | 114.6 (6) | O6ii—O10—V1ii | 77.0 (16) |
O2—V2—O8i | 116.7 (6) | O6ii—O10—V3 | 173.7 (19) |
O2—V2—O11iii | 107.8 (5) | V1—O10—V1ii | 140.0 (7) |
O2—V2—O6 | 104.5 (4) | V1—O10—V3 | 103.0 (6) |
O4ii—V2—O8i | 126.5 (7) | V1ii—O10—V3 | 98.3 (6) |
O4ii—V2—O11iii | 91.6 (6) | O7vii—O11—V4vii | 83.2 (14) |
O4ii—V2—O6 | 76.7 (6) | O7vii—O11—V5 | 69.0 (13) |
O8i—V2—O11iii | 86.4 (6) | V4vii—O11—V5 | 151.5 (9) |
O8i—V2—O6 | 77.2 (6) | N2—Ni—N2ix | 180.0 (3) |
O11iii—V2—O6 | 147.6 (5) | N2—Ni—O1x | 91.9 (2) |
O3—V3—O5ii | 118.2 (6) | N2—Ni—O1i | 88.1 (2) |
O3—V3—O9ii | 117.0 (6) | N2—Ni—N1 | 83.5 (3) |
O3—V3—O7iv | 109.9 (5) | N2—Ni—N1ix | 96.5 (3) |
O3—V3—O10 | 104.1 (5) | N2ix—Ni—O1x | 88.1 (2) |
O5ii—V3—O9ii | 122.6 (7) | N2ix—Ni—O1i | 91.9 (2) |
O5ii—V3—O7iv | 89.1 (6) | N2ix—Ni—N1 | 96.5 (3) |
O5ii—V3—O10 | 77.4 (6) | N2ix—Ni—N1ix | 83.5 (3) |
O9ii—V3—O7iv | 86.1 (6) | O1x—Ni—O1i | 180.0 (2) |
O9ii—V3—O10 | 75.7 (6) | O1x—Ni—N1 | 89.1 (3) |
O7iv—V3—O10 | 145.8 (5) | O1x—Ni—N1ix | 90.9 (3) |
O2i—V4—O11v | 133.0 (5) | O1i—Ni—N1 | 90.9 (3) |
O2i—V4—O7 | 107.3 (5) | O1i—Ni—N1ix | 89.1 (3) |
O2i—V4—O4 | 108.5 (5) | N1—Ni—N1ix | 180.0 (3) |
O2i—V4—O8vi | 111.1 (5) | H2—C1—H1 | 109.07 |
O2i—V4—O6i | 88.0 (4) | H2—C1—N1 | 109.72 |
O11v—V4—O7 | 25.8 (6) | H2—C1—C2 | 108.83 |
O11v—V4—O4 | 99.2 (7) | H1—C1—N1 | 110.05 |
O11v—V4—O8vi | 93.5 (7) | H1—C1—C2 | 109.86 |
O11v—V4—O6i | 138.9 (6) | N1—C1—C2 | 109.3 (8) |
O7—V4—O4 | 110.4 (7) | H3—C2—H4 | 106.79 |
O7—V4—O8vi | 109.9 (6) | H3—C2—N2 | 110.36 |
O7—V4—O6i | 164.7 (6) | H3—C2—C1 | 111.55 |
O4—V4—O8vi | 109.5 (7) | H4—C2—N2 | 109.93 |
O4—V4—O6i | 62.4 (6) | H4—C2—C1 | 110.83 |
O8vi—V4—O6i | 63.5 (5) | N2—C2—C1 | 107.4 (8) |
O7vii—V5—O3i | 132.1 (6) | H6—N1—H5 | 108.50 |
O7vii—V5—O11 | 26.0 (6) | H6—N1—C1 | 110.34 |
O7vii—V5—O5 | 97.2 (7) | H6—N1—Ni | 111.11 |
O7vii—V5—O9 | 95.5 (7) | H5—N1—C1 | 109.57 |
O7vii—V5—O10i | 141.0 (6) | H5—N1—Ni | 110.50 |
O3i—V5—O11 | 106.2 (5) | C1—N1—Ni | 106.8 (6) |
O3i—V5—O5 | 108.9 (5) | H7—N2—H8 | 108.04 |
O3i—V5—O9 | 111.1 (5) | H7—N2—C2 | 109.49 |
O3i—V5—O10i | 86.9 (4) | H7—N2—Ni | 110.18 |
O11—V5—O5 | 109.0 (7) | H8—N2—C2 | 110.79 |
O11—V5—O9 | 111.3 (7) | H8—N2—Ni | 110.08 |
O11—V5—O10i | 166.9 (6) | C2—N2—Ni | 108.3 (5) |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x, −y+1/2, z−1/2; (iii) x−1, −y+1/2, z−1/2; (iv) x+1, −y+1/2, z−1/2; (v) x−1, y, z; (vi) x, y, z+1; (vii) x+1, y, z; (viii) −x+1, y−1/2, −z+1/2; (ix) −x+1, −y+1, −z+1; (x) −x+1, y+1/2, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H5···O2i | 0.960 | 2.101 | 3.044 | 166.99 |
N1—H6···O3ix | 0.949 | 2.366 | 3.157 | 140.59 |
N2—H7···O3xi | 0.956 | 2.280 | 3.163 | 153.16 |
N2—H8···O2ii | 0.958 | 2.491 | 3.036 | 116.01 |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x, −y+1/2, z−1/2; (ix) −x+1, −y+1, −z+1; (xi) −x+1, −y+1, −z. |
(Ordered-en2NiV6O14) bis-ethylenediamine nickel hexavanadium tetradecaoxide top
Crystal data top
(NH2CH2CH2NH2)2NiV6O14 | β = 111.610 (2)° |
Mr = 708.59 | V = 1884.9 (7) Å3 |
Monoclinic, P21/n | Z = 4 |
a = 17.862 (2) Å | F(000) = 1384 |
b = 17.127 (2) Å | Dx = 2.497 Mg m−3 |
c = 6.6270 (8) Å |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Ni1 | 0.5 | 0.5 | 0.5 | 0.0098 (4) | |
Ni1a | 0.5 | 0 | 1 | 0.0098 (4) | |
V1 | 0.50181 (7) | 0.20999 (7) | 0.1424 (2) | 0.0071 (4) | |
V2 | 0.3655 (2) | 0.2133 (2) | 0.2810 (5) | 0.0099 (4) | |
V3 | 0.6387 (2) | 0.2894 (2) | 0.0584 (5) | 0.0107 (4) | |
V4 | 0.3380 (2) | 0.2878 (2) | 0.7532 (5) | 0.0099 (4) | |
V5 | 0.6647 (2) | 0.2133 (2) | 0.5882 (5) | 0.0107 (4) | |
V1a | 0.50181 (7) | 0.29001 (7) | 0.6424 (2) | 0.0071 (4) | |
O1 | 0.5006 (3) | 0.1194 (3) | 0.0690 (8) | 0.013 (2) | |
O2 | 0.3457 (3) | 0.1213 (3) | 0.2816 (9) | 0.017 (2) | |
O3 | 0.6552 (4) | 0.3796 (3) | 0.1123 (9) | 0.018 (2) | |
O4 | 0.3884 (9) | 0.2578 (8) | 0.574 (2) | 0.013 (2) | |
O5 | 0.6177 (9) | 0.2399 (8) | 0.303 (2) | 0.017 (2) | |
O6 | 0.4842 (7) | 0.2191 (7) | 0.404 (2) | 0.016 (2) | |
O7 | 0.2402 (7) | 0.2669 (7) | 0.644 (2) | 0.019 (2) | |
O8 | 0.3843 (9) | 0.2373 (8) | 0.018 (2) | 0.013 (2) | |
O9 | 0.6181 (9) | 0.2686 (8) | 0.752 (2) | 0.017 (2) | |
O10 | 0.5208 (7) | 0.2807 (7) | −0.055 (2) | 0.016 (2) | |
O11 | 0.7631 (7) | 0.2305 (7) | 0.671 (2) | 0.019 (2) | |
O1a | 0.5006 (3) | 0.3806 (3) | 0.5690 (8) | 0.013 (2) | |
O2a | 0.3457 (3) | 0.3787 (3) | 0.7816 (9) | 0.017 (2) | |
O3a | 0.6552 (4) | 0.1204 (3) | 0.6123 (9) | 0.018 (2) | |
N1 | 0.3935 (4) | 0.5160 (4) | 0.5629 (11) | 0.020 (2) | |
N2 | 0.4210 (4) | 0.4757 (4) | 0.1903 (10) | 0.017 (2) | |
N1a | 0.3935 (4) | −0.0160 (4) | 1.0629 (11) | 0.020 (2) | |
N2a | 0.4210 (4) | 0.0243 (4) | 0.6903 (10) | 0.017 (2) | |
C1 | 0.3262 (5) | 0.5164 (6) | 0.3504 (14) | 0.026 (3) | |
C2 | 0.3428 (6) | 0.4566 (6) | 0.201 (2) | 0.029 (3) | |
C1a | 0.3262 (5) | −0.0164 (6) | 0.8504 (14) | 0.026 (3) | |
C2a | 0.3428 (6) | 0.0434 (6) | 0.701 (2) | 0.029 (3) | |
H1 | 0.27699 | 0.50396 | 0.36866 | 0.05066* | |
H2 | 0.32155 | 0.56683 | 0.28603 | 0.05066* | |
H3 | 0.30131 | 0.45748 | 0.05737 | 0.05066* | |
H4 | 0.34380 | 0.40419 | 0.25675 | 0.05066* | |
H5 | 0.38640 | 0.47393 | 0.64993 | 0.05066* | |
H6 | 0.39498 | 0.56364 | 0.63726 | 0.05066* | |
H7 | 0.41555 | 0.52004 | 0.09848 | 0.05066* | |
H8 | 0.44079 | 0.43301 | 0.13069 | 0.05066* | |
H1a | 0.27699 | −0.00396 | 0.86866 | 0.05066* | |
H2a | 0.32155 | −0.06683 | 0.78603 | 0.05066* | |
H3a | 0.30131 | 0.04252 | 0.55737 | 0.05066* | |
H4a | 0.34380 | 0.09581 | 0.75675 | 0.05066* | |
H5a | 0.38640 | 0.02607 | 1.14993 | 0.05066* | |
H6a | 0.39498 | −0.06364 | 1.13726 | 0.05066* | |
H7a | 0.41555 | −0.02004 | 0.59848 | 0.05066* | |
H8a | 0.44079 | 0.06699 | 0.63069 | 0.05066* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0029 (2) | 0.0143 (8) | 0.0116 (8) | −0.0006 (3) | 0.0021 (4) | 0.0011 (6) |
Ni1a | 0.0029 (2) | 0.0143 (8) | 0.0116 (8) | 0.0006 (3) | 0.0021 (4) | −0.0011 (6) |
V1 | 0.0010 (2) | 0.0122 (7) | 0.0077 (7) | 0.0000 (3) | 0.0012 (3) | −0.0002 (5) |
V1a | 0.0010 (2) | 0.0122 (7) | 0.0077 (7) | 0.0000 (3) | 0.0012 (3) | 0.0002 (5) |
O1 | 0.0041 (8) | 0.018 (3) | 0.015 (3) | −0.0018 (13) | 0.0019 (14) | −0.007 (2) |
O2 | 0.0067 (9) | 0.016 (3) | 0.027 (4) | −0.0023 (13) | 0.006 (2) | −0.001 (3) |
O3 | 0.0083 (9) | 0.017 (3) | 0.028 (3) | −0.0024 (14) | 0.007 (2) | −0.005 (3) |
O1a | 0.0041 (8) | 0.018 (3) | 0.015 (3) | 0.0018 (13) | 0.0019 (14) | 0.007 (2) |
O2a | 0.0067 (9) | 0.016 (3) | 0.027 (4) | 0.0023 (13) | 0.006 (2) | 0.001 (3) |
O3a | 0.0083 (9) | 0.017 (3) | 0.028 (3) | 0.0024 (14) | 0.007 (2) | 0.005 (3) |
N1 | 0.0074 (11) | 0.024 (4) | 0.031 (4) | −0.002 (2) | 0.011 (2) | 0.001 (3) |
N2 | 0.0044 (10) | 0.028 (4) | 0.016 (4) | 0.0009 (15) | 0.002 (2) | −0.001 (3) |
N1a | 0.0074 (11) | 0.024 (4) | 0.031 (4) | 0.002 (2) | 0.011 (2) | −0.001 (3) |
N2a | 0.0044 (10) | 0.028 (4) | 0.016 (4) | −0.0009 (15) | 0.002 (2) | 0.001 (3) |
C1 | 0.0016 (13) | 0.045 (7) | 0.026 (6) | 0.002 (2) | −0.001 (3) | 0.007 (5) |
C2 | 0.0021 (13) | 0.050 (7) | 0.025 (6) | −0.002 (2) | −0.006 (3) | 0.000 (5) |
C1a | 0.0016 (13) | 0.045 (7) | 0.026 (6) | −0.002 (2) | −0.001 (3) | −0.007 (5) |
C2a | 0.0021 (13) | 0.050 (7) | 0.025 (6) | 0.002 (2) | −0.006 (3) | 0.000 (5) |
Geometric parameters (Å, º) top
Ni1—N2 | 2.060 (6) | V5—O3a | 1.614 (6) |
Ni1—N2i | 2.060 (6) | V5—O11 | 1.663 (14) |
Ni1—O1a | 2.095 (5) | V5—O5 | 1.823 (13) |
Ni1—O1ai | 2.095 (5) | V5—O9 | 1.853 (15) |
Ni1—N1 | 2.109 (8) | V1a—O1a | 1.624 (5) |
Ni1—N1i | 2.109 (8) | V1a—O10iii | 1.916 (12) |
Ni1a—N2a | 2.060 (6) | V1a—O6 | 1.927 (12) |
Ni1a—N2aii | 2.060 (6) | V1a—O9 | 1.97 (2) |
Ni1a—O1iii | 2.095 (5) | V1a—O4 | 1.98 (2) |
Ni1a—O1iv | 2.095 (5) | N1—H6 | 0.949 |
Ni1a—N1a | 2.109 (8) | N1—H5 | 0.960 |
Ni1a—N1aii | 2.109 (8) | N1—C1 | 1.477 (11) |
V1—O1 | 1.624 (5) | N2—H7 | 0.956 |
V1—O6 | 1.876 (13) | N2—H8 | 0.958 |
V1—O10 | 1.900 (13) | N2—C2 | 1.461 (14) |
V1—O8 | 2.01 (2) | N1a—H6a | 0.949 |
V1—O5 | 2.01 (2) | N1a—H5a | 0.960 |
V2—O2 | 1.617 (6) | N1a—C1a | 1.477 (11) |
V2—O8 | 1.934 (14) | N2a—H7a | 0.956 |
V2—O11v | 1.955 (14) | N2a—H8a | 0.958 |
V2—O6 | 1.973 (14) | N2a—C2a | 1.461 (14) |
V2—O4 | 1.983 (13) | C1—H2 | 0.953 |
V3—O3 | 1.590 (6) | C1—H1 | 0.954 |
V3—O7vi | 1.944 (14) | C1—C2 | 1.527 (15) |
V3—O9vii | 1.958 (13) | C2—H3 | 0.967 |
V3—O10 | 1.963 (14) | C2—H4 | 0.969 |
V3—O5 | 1.981 (14) | C1a—H2a | 0.953 |
V4—O2a | 1.569 (6) | C1a—H1a | 0.954 |
V4—O7 | 1.666 (14) | C1a—C2a | 1.527 (15) |
V4—O4 | 1.809 (15) | C2a—H3a | 0.967 |
V4—O8iii | 1.857 (13) | C2a—H4a | 0.969 |
N2—Ni1—N2i | 180.0 (3) | O10iii—V1a—O6 | 136.1 (5) |
N2—Ni1—O1a | 88.1 (2) | O10iii—V1a—O9 | 80.9 (6) |
N2—Ni1—O1ai | 91.9 (2) | O10iii—V1a—O4 | 89.3 (6) |
N2—Ni1—N1 | 83.5 (3) | O6—V1a—O9 | 91.0 (6) |
N2—Ni1—N1i | 96.5 (3) | O6—V1a—O4 | 78.0 (6) |
N2i—Ni1—O1a | 91.9 (2) | O9—V1a—O4 | 152.0 (6) |
N2i—Ni1—O1ai | 88.1 (2) | V1—O1—Ni1avii | 175.3 (3) |
N2i—Ni1—N1 | 96.5 (3) | V4—O4—V2 | 141.2 (8) |
N2i—Ni1—N1i | 83.5 (3) | V4—O4—V1a | 118.9 (8) |
O1a—Ni1—O1ai | 180.0 (2) | V2—O4—V1a | 99.0 (6) |
O1a—Ni1—N1 | 90.9 (2) | V5—O5—V3 | 143.3 (8) |
O1a—Ni1—N1i | 89.1 (2) | V5—O5—V1 | 118.3 (8) |
O1ai—Ni1—N1 | 89.1 (2) | V3—O5—V1 | 98.4 (6) |
O1ai—Ni1—N1i | 90.9 (2) | V1—O6—V1a | 141.1 (7) |
N1—Ni1—N1i | 180.0 (3) | V1—O6—V2 | 97.8 (6) |
N2a—Ni1a—N2aii | 180.0 (3) | V1a—O6—V2 | 101.3 (6) |
N2a—Ni1a—O1iii | 88.1 (2) | V4—O7—V3viii | 161.7 (8) |
N2a—Ni1a—O1iv | 91.9 (2) | V4vii—O8—V2 | 141.8 (8) |
N2a—Ni1a—N1a | 83.5 (3) | V4vii—O8—V1 | 122.0 (8) |
N2a—Ni1a—N1aii | 96.5 (3) | V2—O8—V1 | 94.8 (6) |
N2aii—Ni1a—O1iii | 91.9 (2) | V5—O9—V3iii | 138.3 (8) |
N2aii—Ni1a—O1iv | 88.1 (2) | V5—O9—V1a | 121.4 (8) |
N2aii—Ni1a—N1a | 96.5 (3) | V3iii—O9—V1a | 96.8 (6) |
N2aii—Ni1a—N1aii | 83.5 (3) | V1—O10—V1avii | 140.0 (7) |
O1iii—Ni1a—O1iv | 180.0 (2) | V1—O10—V3 | 103.0 (6) |
O1iii—Ni1a—N1a | 90.9 (2) | V1avii—O10—V3 | 98.3 (6) |
O1iii—Ni1a—N1aii | 89.1 (2) | V5—O11—V2ix | 160.1 (8) |
O1iv—Ni1a—N1a | 89.1 (2) | V1a—O1a—Ni1 | 175.3 (3) |
O1iv—Ni1a—N1aii | 90.9 (2) | H6—N1—H5 | 108.51 |
N1a—Ni1a—N1aii | 180.0 (3) | H6—N1—C1 | 110.34 |
O1—V1—O6 | 111.6 (4) | H6—N1—Ni1 | 111.11 |
O1—V1—O10 | 112.9 (4) | H5—N1—C1 | 109.56 |
O1—V1—O8 | 101.7 (5) | H5—N1—Ni1 | 110.50 |
O1—V1—O5 | 107.4 (5) | C1—N1—Ni1 | 106.8 (5) |
O6—V1—O10 | 135.5 (6) | H7—N2—H8 | 108.04 |
O6—V1—O8 | 81.5 (6) | H7—N2—C2 | 109.49 |
O6—V1—O5 | 89.0 (6) | H7—N2—Ni1 | 110.18 |
O10—V1—O8 | 89.7 (6) | H8—N2—C2 | 110.79 |
O10—V1—O5 | 77.9 (6) | H8—N2—Ni1 | 110.08 |
O8—V1—O5 | 150.9 (6) | C2—N2—Ni1 | 108.3 (6) |
O2—V2—O8 | 108.6 (5) | H6a—N1a—H5a | 108.51 |
O2—V2—O11v | 107.8 (5) | H6a—N1a—C1a | 110.34 |
O2—V2—O6 | 104.5 (5) | H6a—N1a—Ni1a | 111.11 |
O2—V2—O4 | 109.8 (5) | H5a—N1a—C1a | 109.56 |
O8—V2—O11v | 90.5 (6) | H5a—N1a—Ni1a | 110.50 |
O8—V2—O6 | 81.0 (6) | C1a—N1a—Ni1a | 106.8 (5) |
O8—V2—O4 | 139.3 (6) | H7a—N2a—H8a | 108.04 |
O11v—V2—O6 | 147.6 (6) | H7a—N2a—C2a | 109.49 |
O11v—V2—O4 | 90.1 (6) | H7a—N2a—Ni1a | 110.18 |
O6—V2—O4 | 77.0 (6) | H8a—N2a—C2a | 110.79 |
O3—V3—O7vi | 109.9 (5) | H8a—N2a—Ni1a | 110.08 |
O3—V3—O9vii | 111.0 (5) | C2a—N2a—Ni1a | 108.3 (6) |
O3—V3—O10 | 104.1 (5) | H2—C1—H1 | 109.07 |
O3—V3—O5 | 107.9 (5) | H2—C1—N1 | 109.72 |
O7vi—V3—O9vii | 90.6 (6) | H2—C1—C2 | 108.82 |
O7vi—V3—O10 | 145.8 (6) | H1—C1—N1 | 110.05 |
O7vi—V3—O5 | 89.2 (6) | H1—C1—C2 | 109.86 |
O9vii—V3—O10 | 79.9 (6) | N1—C1—C2 | 109.3 (8) |
O9vii—V3—O5 | 138.5 (6) | H3—C2—H4 | 106.79 |
O10—V3—O5 | 77.3 (6) | H3—C2—N2 | 110.36 |
O2a—V4—O7 | 107.3 (5) | H3—C2—C1 | 111.55 |
O2a—V4—O4 | 108.5 (5) | H4—C2—N2 | 109.93 |
O2a—V4—O8iii | 111.1 (5) | H4—C2—C1 | 110.83 |
O7—V4—O4 | 110.4 (7) | N2—C2—C1 | 107.4 (8) |
O7—V4—O8iii | 109.9 (7) | H2a—C1a—H1a | 109.07 |
O4—V4—O8iii | 109.5 (7) | H2a—C1a—N1a | 109.72 |
O3a—V5—O11 | 106.2 (5) | H2a—C1a—C2a | 108.82 |
O3a—V5—O5 | 108.9 (5) | H1a—C1a—N1a | 110.05 |
O3a—V5—O9 | 111.1 (5) | H1a—C1a—C2a | 109.86 |
O11—V5—O5 | 109.0 (7) | N1a—C1a—C2a | 109.3 (8) |
O11—V5—O9 | 111.3 (7) | H3a—C2a—H4a | 106.79 |
O5—V5—O9 | 110.2 (7) | H3a—C2a—N2a | 110.36 |
O1a—V1a—O10iii | 111.8 (4) | H3a—C2a—C1a | 111.55 |
O1a—V1a—O6 | 112.1 (4) | H4a—C2a—N2a | 109.93 |
O1a—V1a—O9 | 100.7 (5) | H4a—C2a—C1a | 110.83 |
O1a—V1a—O4 | 107.3 (5) | N2a—C2a—C1a | 107.4 (8) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z+2; (iii) x, y, z+1; (iv) −x+1, −y, −z+1; (v) x−1/2, −y+1/2, z−1/2; (vi) x+1/2, −y+1/2, z−1/2; (vii) x, y, z−1; (viii) x−1/2, −y+1/2, z+1/2; (ix) x+1/2, −y+1/2, z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H5···O2a | 0.960 | 2.101 | 3.044 | 166.99 |
N1—H6···O3i | 0.949 | 2.366 | 3.157 | 140.59 |
N2—H7···O3x | 0.956 | 2.280 | 3.163 | 153.16 |
N2—H8···O2avii | 0.958 | 2.491 | 3.036 | 116.01 |
N1a—H5a···O2iii | 0.960 | 2.101 | 3.044 | 166.99 |
N1a—H6a···O3aii | 0.949 | 2.366 | 3.157 | 140.59 |
N2a—H7a···O3aiv | 0.956 | 2.280 | 3.163 | 153.16 |
N2a—H8a···O2 | 0.958 | 2.491 | 3.036 | 116.01 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y, −z+2; (iii) x, y, z+1; (iv) −x+1, −y, −z+1; (vii) x, y, z−1; (x) −x+1, −y+1, −z. |