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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

cif

Crystallographic Information File (CIF)
Contains datablocks global, OD-en2NiV6O14, Ordered-en2NiV6O14

hkl

Structure factor file (CIF format)
Contains datablock OD-en2NiV6O14

hkl

Structure factor file (CIF format)
Contains datablock Ordered-en2NiV6O14

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)2NiV6O14F(000) = 692
Mr = 708.59Dx = 2.497 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 8.9311 (11) ÅCell parameters from 1430 reflections
b = 17.127 (2) Åθ = 4.7–28°
c = 6.6270 (8) ŵ = 3.90 mm1
β = 111.610 (2)°T = 295 K
V = 942.4 (3) Å3Plate, black
Z = 20.41 × 0.16 × 0.06 mm
Data collection top
Siemens Smart CCD
diffractometer
1684 independent reflections
Radiation source: sealed tube1267 reflections with Fo > 4σ(Fo)
Graphite monochromatorRint = 0.051
ω scansθmax = 28°, θmin = 3.1°
Absorption correction: multi-scan SADABS (sheldrick, 1996)h = 82
Tmin = 0.641, Tmax = 0.777k = 114
3679 measured reflectionsl = 2120
Refinement top
Refinement on FH-atom parameters not refined
Least-squares matrix: full with fixed elements per cyclew = 1/[σ(Fo)2 + 0.002Fo2)]
R[F2 > 2σ(F2)] = 0.060(Δ/σ)max = 0.01
wR(F2) = 0.0637Δρmax = 0.93 e Å3
1267 reflectionsΔρmin = 1.22 e Å3
165 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
V10.50362 (1)0.20999 (7)0.1424 (2)0.0079 (5)
V20.2310 (3)0.2133 (2)0.2810 (5)0.0099 (4)0.5
V30.7774 (3)0.2894 (2)0.0584 (5)0.0107 (4)0.5
V40.1761 (3)0.2878 (2)0.7532 (5)0.0099 (4)0.5
V50.8294 (3)0.2133 (2)0.5882 (5)0.0107 (4)0.5
O10.5012 (6)0.1194 (3)0.0690 (8)0.017 (2)
O20.1915 (7)0.1213 (3)0.2816 (9)0.023 (2)
O30.8104 (7)0.3796 (3)0.1123 (9)0.025 (2)
O40.277 (2)0.2578 (8)0.574 (2)0.013 (2)0.5
O50.735 (2)0.2399 (8)0.303 (2)0.017 (2)0.5
O60.4683 (14)0.2191 (7)0.404 (2)0.016 (2)0.5
O70.0196 (14)0.2669 (7)0.644 (2)0.019 (2)0.5
O80.269 (2)0.2373 (8)0.018 (2)0.013 (2)0.5
O90.736 (2)0.2686 (8)0.752 (2)0.017 (2)0.5
O100.5417 (14)0.2807 (7)0.055 (2)0.016 (2)0.5
O111.0262 (14)0.2304 (7)0.671 (2)0.019 (2)0.5
Ni0.50.50.50.0125 (6)
C10.1524 (10)0.5164 (6)0.3504 (14)0.028 (4)
C20.1855 (11)0.4566 (6)0.201 (2)0.033 (4)
N10.2871 (9)0.5160 (4)0.5629 (11)0.025 (3)
N20.3419 (8)0.4757 (4)0.1903 (10)0.021 (3)
H10.053980.503960.368660.05066*
H20.143100.566830.286030.05066*
H30.102620.457480.057370.05066*
H40.187600.404190.256750.05066*
H50.272800.473930.649930.05066*
H60.289960.563640.637260.05066*
H70.331090.520040.098480.05066*
H80.381570.433010.130690.05066*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
V10.0041 (7)0.0121 (7)0.0077 (7)0.0000 (5)0.0023 (7)0.0002 (5)
O10.016 (3)0.018 (3)0.015 (3)0.004 (2)0.004 (3)0.007 (2)
O20.027 (4)0.016 (3)0.027 (4)0.005 (3)0.012 (3)0.001 (3)
O30.033 (4)0.017 (3)0.028 (3)0.005 (3)0.014 (3)0.005 (3)
Ni0.0115 (8)0.0142 (8)0.0116 (8)0.0012 (6)0.0041 (7)0.0011 (6)
C10.006 (5)0.045 (7)0.026 (6)0.004 (4)0.001 (5)0.007 (5)
C20.008 (5)0.050 (7)0.025 (6)0.003 (5)0.012 (5)0.000 (5)
N10.030 (4)0.024 (4)0.031 (4)0.004 (3)0.022 (4)0.001 (3)
N20.018 (4)0.028 (4)0.016 (4)0.002 (3)0.003 (4)0.001 (3)
Geometric parameters (Å, º) top
V1—O11.624 (6)V5—O7vii1.559 (13)
V1—O61.876 (12)V5—O3i1.614 (7)
V1—O101.900 (12)V5—O111.663 (14)
V1—O10i1.916 (12)V5—O51.823 (13)
V1—O6ii1.927 (12)V5—O91.853 (15)
V1—O9ii1.97 (2)V5—O10i2.392 (13)
V1—O4ii1.98 (2)O1—Niviii2.095 (5)
V1—O82.01 (2)O6—O10i0.61 (2)
V2—O21.617 (6)O7—O11v0.73 (2)
V2—O4ii1.646 (14)Ni—N22.060 (6)
V2—O8i1.707 (13)Ni—N2ix2.060 (6)
V2—O11iii1.955 (13)Ni—N12.109 (8)
V2—O61.973 (13)Ni—N1ix2.109 (8)
V3—O31.590 (7)C1—H20.953
V3—O5ii1.673 (13)C1—H10.954
V3—O9ii1.765 (15)C1—N11.477 (12)
V3—O7iv1.944 (13)C1—C21.527 (14)
V3—O101.963 (13)C2—H30.967
V4—O2i1.569 (6)C2—H40.969
V4—O11v1.586 (13)C2—N21.461 (13)
V4—O71.666 (13)N1—H60.949
V4—O41.809 (15)N1—H50.960
V4—O8vi1.857 (13)N2—H70.956
V4—O6i2.430 (13)N2—H80.958
O1—V1—O6111.6 (4)O5—V5—O9110.2 (7)
O1—V1—O10112.9 (4)O5—V5—O10i64.0 (6)
O1—V1—O10i111.8 (4)O9—V5—O10i63.9 (6)
O1—V1—O6ii112.1 (4)V1—O1—Niviii175.3 (3)
O1—V1—O9ii100.6 (5)V4ii—O2—V216.4 (2)
O1—V1—O4ii107.3 (5)V3—O3—V5ii15.6 (2)
O1—V1—O8101.7 (5)V2i—O4—V2155.1 (9)
O6—V1—O10135.5 (5)V2i—O4—V1i105.8 (7)
O6—V1—O10i18.5 (5)V2—O4—V1i99.0 (6)
O6—V1—O6ii132.3 (5)V3i—O5—V3156.4 (9)
O6—V1—O9ii99.1 (6)V3i—O5—V1105.2 (7)
O6—V1—O4ii71.6 (6)V3—O5—V198.4 (6)
O6—V1—O881.5 (6)O10i—O6—V184.5 (16)
O10—V1—O10i131.2 (5)O10i—O6—V1i78.4 (16)
O10—V1—O6ii18.3 (5)O10i—O6—V2176.4 (19)
O10—V1—O9ii72.7 (6)V1—O6—V1i141.1 (7)
O10—V1—O4ii95.2 (6)V1—O6—V297.8 (6)
O10—V1—O889.7 (6)V1i—O6—V2101.3 (6)
O10i—V1—O6ii136.1 (5)O11v—O7—V5v85.0 (14)
O10i—V1—O9ii80.9 (6)O11v—O7—V471.0 (14)
O10i—V1—O4ii89.3 (6)V5v—O7—V4155.1 (9)
O10i—V1—O899.5 (6)V2ii—O8—V2153.4 (9)
O6ii—V1—O9ii91.0 (6)V2ii—O8—V1108.3 (7)
O6ii—V1—O4ii78.0 (6)V2—O8—V194.8 (6)
O6ii—V1—O871.7 (6)V3i—O9—V3vi147.8 (9)
O9ii—V1—O4ii152.0 (6)V3i—O9—V1i108.2 (7)
O9ii—V1—O8155.6 (6)V3vi—O9—V1i96.8 (7)
O4ii—V1—O810.3 (6)O6ii—O10—V183.3 (16)
O2—V2—O4ii114.6 (6)O6ii—O10—V1ii77.0 (16)
O2—V2—O8i116.7 (6)O6ii—O10—V3173.7 (19)
O2—V2—O11iii107.8 (5)V1—O10—V1ii140.0 (7)
O2—V2—O6104.5 (4)V1—O10—V3103.0 (6)
O4ii—V2—O8i126.5 (7)V1ii—O10—V398.3 (6)
O4ii—V2—O11iii91.6 (6)O7vii—O11—V4vii83.2 (14)
O4ii—V2—O676.7 (6)O7vii—O11—V569.0 (13)
O8i—V2—O11iii86.4 (6)V4vii—O11—V5151.5 (9)
O8i—V2—O677.2 (6)N2—Ni—N2ix180.0 (3)
O11iii—V2—O6147.6 (5)N2—Ni—O1x91.9 (2)
O3—V3—O5ii118.2 (6)N2—Ni—O1i88.1 (2)
O3—V3—O9ii117.0 (6)N2—Ni—N183.5 (3)
O3—V3—O7iv109.9 (5)N2—Ni—N1ix96.5 (3)
O3—V3—O10104.1 (5)N2ix—Ni—O1x88.1 (2)
O5ii—V3—O9ii122.6 (7)N2ix—Ni—O1i91.9 (2)
O5ii—V3—O7iv89.1 (6)N2ix—Ni—N196.5 (3)
O5ii—V3—O1077.4 (6)N2ix—Ni—N1ix83.5 (3)
O9ii—V3—O7iv86.1 (6)O1x—Ni—O1i180.0 (2)
O9ii—V3—O1075.7 (6)O1x—Ni—N189.1 (3)
O7iv—V3—O10145.8 (5)O1x—Ni—N1ix90.9 (3)
O2i—V4—O11v133.0 (5)O1i—Ni—N190.9 (3)
O2i—V4—O7107.3 (5)O1i—Ni—N1ix89.1 (3)
O2i—V4—O4108.5 (5)N1—Ni—N1ix180.0 (3)
O2i—V4—O8vi111.1 (5)H2—C1—H1109.07
O2i—V4—O6i88.0 (4)H2—C1—N1109.72
O11v—V4—O725.8 (6)H2—C1—C2108.83
O11v—V4—O499.2 (7)H1—C1—N1110.05
O11v—V4—O8vi93.5 (7)H1—C1—C2109.86
O11v—V4—O6i138.9 (6)N1—C1—C2109.3 (8)
O7—V4—O4110.4 (7)H3—C2—H4106.79
O7—V4—O8vi109.9 (6)H3—C2—N2110.36
O7—V4—O6i164.7 (6)H3—C2—C1111.55
O4—V4—O8vi109.5 (7)H4—C2—N2109.93
O4—V4—O6i62.4 (6)H4—C2—C1110.83
O8vi—V4—O6i63.5 (5)N2—C2—C1107.4 (8)
O7vii—V5—O3i132.1 (6)H6—N1—H5108.50
O7vii—V5—O1126.0 (6)H6—N1—C1110.34
O7vii—V5—O597.2 (7)H6—N1—Ni111.11
O7vii—V5—O995.5 (7)H5—N1—C1109.57
O7vii—V5—O10i141.0 (6)H5—N1—Ni110.50
O3i—V5—O11106.2 (5)C1—N1—Ni106.8 (6)
O3i—V5—O5108.9 (5)H7—N2—H8108.04
O3i—V5—O9111.1 (5)H7—N2—C2109.49
O3i—V5—O10i86.9 (4)H7—N2—Ni110.18
O11—V5—O5109.0 (7)H8—N2—C2110.79
O11—V5—O9111.3 (7)H8—N2—Ni110.08
O11—V5—O10i166.9 (6)C2—N2—Ni108.3 (5)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (iii) x1, y+1/2, z1/2; (iv) x+1, y+1/2, z1/2; (v) x1, y, z; (vi) x, y, z+1; (vii) x+1, y, z; (viii) x+1, y1/2, 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···AD—HH···AD···AD—H···A
N1—H5···O2i0.9602.1013.044166.99
N1—H6···O3ix0.9492.3663.157140.59
N2—H7···O3xi0.9562.2803.163153.16
N2—H8···O2ii0.9582.4913.036116.01
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x, y+1/2, z1/2; (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)2NiV6O14β = 111.610 (2)°
Mr = 708.59V = 1884.9 (7) Å3
Monoclinic, P21/nZ = 4
a = 17.862 (2) ÅF(000) = 1384
b = 17.127 (2) ÅDx = 2.497 Mg m3
c = 6.6270 (8) Å
Data collection top
h = l =
k =
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.50.50.50.0098 (4)
Ni1a0.5010.0098 (4)
V10.50181 (7)0.20999 (7)0.1424 (2)0.0071 (4)
V20.3655 (2)0.2133 (2)0.2810 (5)0.0099 (4)
V30.6387 (2)0.2894 (2)0.0584 (5)0.0107 (4)
V40.3380 (2)0.2878 (2)0.7532 (5)0.0099 (4)
V50.6647 (2)0.2133 (2)0.5882 (5)0.0107 (4)
V1a0.50181 (7)0.29001 (7)0.6424 (2)0.0071 (4)
O10.5006 (3)0.1194 (3)0.0690 (8)0.013 (2)
O20.3457 (3)0.1213 (3)0.2816 (9)0.017 (2)
O30.6552 (4)0.3796 (3)0.1123 (9)0.018 (2)
O40.3884 (9)0.2578 (8)0.574 (2)0.013 (2)
O50.6177 (9)0.2399 (8)0.303 (2)0.017 (2)
O60.4842 (7)0.2191 (7)0.404 (2)0.016 (2)
O70.2402 (7)0.2669 (7)0.644 (2)0.019 (2)
O80.3843 (9)0.2373 (8)0.018 (2)0.013 (2)
O90.6181 (9)0.2686 (8)0.752 (2)0.017 (2)
O100.5208 (7)0.2807 (7)0.055 (2)0.016 (2)
O110.7631 (7)0.2305 (7)0.671 (2)0.019 (2)
O1a0.5006 (3)0.3806 (3)0.5690 (8)0.013 (2)
O2a0.3457 (3)0.3787 (3)0.7816 (9)0.017 (2)
O3a0.6552 (4)0.1204 (3)0.6123 (9)0.018 (2)
N10.3935 (4)0.5160 (4)0.5629 (11)0.020 (2)
N20.4210 (4)0.4757 (4)0.1903 (10)0.017 (2)
N1a0.3935 (4)0.0160 (4)1.0629 (11)0.020 (2)
N2a0.4210 (4)0.0243 (4)0.6903 (10)0.017 (2)
C10.3262 (5)0.5164 (6)0.3504 (14)0.026 (3)
C20.3428 (6)0.4566 (6)0.201 (2)0.029 (3)
C1a0.3262 (5)0.0164 (6)0.8504 (14)0.026 (3)
C2a0.3428 (6)0.0434 (6)0.701 (2)0.029 (3)
H10.276990.503960.368660.05066*
H20.321550.566830.286030.05066*
H30.301310.457480.057370.05066*
H40.343800.404190.256750.05066*
H50.386400.473930.649930.05066*
H60.394980.563640.637260.05066*
H70.415550.520040.098480.05066*
H80.440790.433010.130690.05066*
H1a0.276990.003960.868660.05066*
H2a0.321550.066830.786030.05066*
H3a0.301310.042520.557370.05066*
H4a0.343800.095810.756750.05066*
H5a0.386400.026071.149930.05066*
H6a0.394980.063641.137260.05066*
H7a0.415550.020040.598480.05066*
H8a0.440790.066990.630690.05066*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0029 (2)0.0143 (8)0.0116 (8)0.0006 (3)0.0021 (4)0.0011 (6)
Ni1a0.0029 (2)0.0143 (8)0.0116 (8)0.0006 (3)0.0021 (4)0.0011 (6)
V10.0010 (2)0.0122 (7)0.0077 (7)0.0000 (3)0.0012 (3)0.0002 (5)
V1a0.0010 (2)0.0122 (7)0.0077 (7)0.0000 (3)0.0012 (3)0.0002 (5)
O10.0041 (8)0.018 (3)0.015 (3)0.0018 (13)0.0019 (14)0.007 (2)
O20.0067 (9)0.016 (3)0.027 (4)0.0023 (13)0.006 (2)0.001 (3)
O30.0083 (9)0.017 (3)0.028 (3)0.0024 (14)0.007 (2)0.005 (3)
O1a0.0041 (8)0.018 (3)0.015 (3)0.0018 (13)0.0019 (14)0.007 (2)
O2a0.0067 (9)0.016 (3)0.027 (4)0.0023 (13)0.006 (2)0.001 (3)
O3a0.0083 (9)0.017 (3)0.028 (3)0.0024 (14)0.007 (2)0.005 (3)
N10.0074 (11)0.024 (4)0.031 (4)0.002 (2)0.011 (2)0.001 (3)
N20.0044 (10)0.028 (4)0.016 (4)0.0009 (15)0.002 (2)0.001 (3)
N1a0.0074 (11)0.024 (4)0.031 (4)0.002 (2)0.011 (2)0.001 (3)
N2a0.0044 (10)0.028 (4)0.016 (4)0.0009 (15)0.002 (2)0.001 (3)
C10.0016 (13)0.045 (7)0.026 (6)0.002 (2)0.001 (3)0.007 (5)
C20.0021 (13)0.050 (7)0.025 (6)0.002 (2)0.006 (3)0.000 (5)
C1a0.0016 (13)0.045 (7)0.026 (6)0.002 (2)0.001 (3)0.007 (5)
C2a0.0021 (13)0.050 (7)0.025 (6)0.002 (2)0.006 (3)0.000 (5)
Geometric parameters (Å, º) top
Ni1—N22.060 (6)V5—O3a1.614 (6)
Ni1—N2i2.060 (6)V5—O111.663 (14)
Ni1—O1a2.095 (5)V5—O51.823 (13)
Ni1—O1ai2.095 (5)V5—O91.853 (15)
Ni1—N12.109 (8)V1a—O1a1.624 (5)
Ni1—N1i2.109 (8)V1a—O10iii1.916 (12)
Ni1a—N2a2.060 (6)V1a—O61.927 (12)
Ni1a—N2aii2.060 (6)V1a—O91.97 (2)
Ni1a—O1iii2.095 (5)V1a—O41.98 (2)
Ni1a—O1iv2.095 (5)N1—H60.949
Ni1a—N1a2.109 (8)N1—H50.960
Ni1a—N1aii2.109 (8)N1—C11.477 (11)
V1—O11.624 (5)N2—H70.956
V1—O61.876 (13)N2—H80.958
V1—O101.900 (13)N2—C21.461 (14)
V1—O82.01 (2)N1a—H6a0.949
V1—O52.01 (2)N1a—H5a0.960
V2—O21.617 (6)N1a—C1a1.477 (11)
V2—O81.934 (14)N2a—H7a0.956
V2—O11v1.955 (14)N2a—H8a0.958
V2—O61.973 (14)N2a—C2a1.461 (14)
V2—O41.983 (13)C1—H20.953
V3—O31.590 (6)C1—H10.954
V3—O7vi1.944 (14)C1—C21.527 (15)
V3—O9vii1.958 (13)C2—H30.967
V3—O101.963 (14)C2—H40.969
V3—O51.981 (14)C1a—H2a0.953
V4—O2a1.569 (6)C1a—H1a0.954
V4—O71.666 (14)C1a—C2a1.527 (15)
V4—O41.809 (15)C2a—H3a0.967
V4—O8iii1.857 (13)C2a—H4a0.969
N2—Ni1—N2i180.0 (3)O10iii—V1a—O6136.1 (5)
N2—Ni1—O1a88.1 (2)O10iii—V1a—O980.9 (6)
N2—Ni1—O1ai91.9 (2)O10iii—V1a—O489.3 (6)
N2—Ni1—N183.5 (3)O6—V1a—O991.0 (6)
N2—Ni1—N1i96.5 (3)O6—V1a—O478.0 (6)
N2i—Ni1—O1a91.9 (2)O9—V1a—O4152.0 (6)
N2i—Ni1—O1ai88.1 (2)V1—O1—Ni1avii175.3 (3)
N2i—Ni1—N196.5 (3)V4—O4—V2141.2 (8)
N2i—Ni1—N1i83.5 (3)V4—O4—V1a118.9 (8)
O1a—Ni1—O1ai180.0 (2)V2—O4—V1a99.0 (6)
O1a—Ni1—N190.9 (2)V5—O5—V3143.3 (8)
O1a—Ni1—N1i89.1 (2)V5—O5—V1118.3 (8)
O1ai—Ni1—N189.1 (2)V3—O5—V198.4 (6)
O1ai—Ni1—N1i90.9 (2)V1—O6—V1a141.1 (7)
N1—Ni1—N1i180.0 (3)V1—O6—V297.8 (6)
N2a—Ni1a—N2aii180.0 (3)V1a—O6—V2101.3 (6)
N2a—Ni1a—O1iii88.1 (2)V4—O7—V3viii161.7 (8)
N2a—Ni1a—O1iv91.9 (2)V4vii—O8—V2141.8 (8)
N2a—Ni1a—N1a83.5 (3)V4vii—O8—V1122.0 (8)
N2a—Ni1a—N1aii96.5 (3)V2—O8—V194.8 (6)
N2aii—Ni1a—O1iii91.9 (2)V5—O9—V3iii138.3 (8)
N2aii—Ni1a—O1iv88.1 (2)V5—O9—V1a121.4 (8)
N2aii—Ni1a—N1a96.5 (3)V3iii—O9—V1a96.8 (6)
N2aii—Ni1a—N1aii83.5 (3)V1—O10—V1avii140.0 (7)
O1iii—Ni1a—O1iv180.0 (2)V1—O10—V3103.0 (6)
O1iii—Ni1a—N1a90.9 (2)V1avii—O10—V398.3 (6)
O1iii—Ni1a—N1aii89.1 (2)V5—O11—V2ix160.1 (8)
O1iv—Ni1a—N1a89.1 (2)V1a—O1a—Ni1175.3 (3)
O1iv—Ni1a—N1aii90.9 (2)H6—N1—H5108.51
N1a—Ni1a—N1aii180.0 (3)H6—N1—C1110.34
O1—V1—O6111.6 (4)H6—N1—Ni1111.11
O1—V1—O10112.9 (4)H5—N1—C1109.56
O1—V1—O8101.7 (5)H5—N1—Ni1110.50
O1—V1—O5107.4 (5)C1—N1—Ni1106.8 (5)
O6—V1—O10135.5 (6)H7—N2—H8108.04
O6—V1—O881.5 (6)H7—N2—C2109.49
O6—V1—O589.0 (6)H7—N2—Ni1110.18
O10—V1—O889.7 (6)H8—N2—C2110.79
O10—V1—O577.9 (6)H8—N2—Ni1110.08
O8—V1—O5150.9 (6)C2—N2—Ni1108.3 (6)
O2—V2—O8108.6 (5)H6a—N1a—H5a108.51
O2—V2—O11v107.8 (5)H6a—N1a—C1a110.34
O2—V2—O6104.5 (5)H6a—N1a—Ni1a111.11
O2—V2—O4109.8 (5)H5a—N1a—C1a109.56
O8—V2—O11v90.5 (6)H5a—N1a—Ni1a110.50
O8—V2—O681.0 (6)C1a—N1a—Ni1a106.8 (5)
O8—V2—O4139.3 (6)H7a—N2a—H8a108.04
O11v—V2—O6147.6 (6)H7a—N2a—C2a109.49
O11v—V2—O490.1 (6)H7a—N2a—Ni1a110.18
O6—V2—O477.0 (6)H8a—N2a—C2a110.79
O3—V3—O7vi109.9 (5)H8a—N2a—Ni1a110.08
O3—V3—O9vii111.0 (5)C2a—N2a—Ni1a108.3 (6)
O3—V3—O10104.1 (5)H2—C1—H1109.07
O3—V3—O5107.9 (5)H2—C1—N1109.72
O7vi—V3—O9vii90.6 (6)H2—C1—C2108.82
O7vi—V3—O10145.8 (6)H1—C1—N1110.05
O7vi—V3—O589.2 (6)H1—C1—C2109.86
O9vii—V3—O1079.9 (6)N1—C1—C2109.3 (8)
O9vii—V3—O5138.5 (6)H3—C2—H4106.79
O10—V3—O577.3 (6)H3—C2—N2110.36
O2a—V4—O7107.3 (5)H3—C2—C1111.55
O2a—V4—O4108.5 (5)H4—C2—N2109.93
O2a—V4—O8iii111.1 (5)H4—C2—C1110.83
O7—V4—O4110.4 (7)N2—C2—C1107.4 (8)
O7—V4—O8iii109.9 (7)H2a—C1a—H1a109.07
O4—V4—O8iii109.5 (7)H2a—C1a—N1a109.72
O3a—V5—O11106.2 (5)H2a—C1a—C2a108.82
O3a—V5—O5108.9 (5)H1a—C1a—N1a110.05
O3a—V5—O9111.1 (5)H1a—C1a—C2a109.86
O11—V5—O5109.0 (7)N1a—C1a—C2a109.3 (8)
O11—V5—O9111.3 (7)H3a—C2a—H4a106.79
O5—V5—O9110.2 (7)H3a—C2a—N2a110.36
O1a—V1a—O10iii111.8 (4)H3a—C2a—C1a111.55
O1a—V1a—O6112.1 (4)H4a—C2a—N2a109.93
O1a—V1a—O9100.7 (5)H4a—C2a—C1a110.83
O1a—V1a—O4107.3 (5)N2a—C2a—C1a107.4 (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) x1/2, y+1/2, z1/2; (vi) x+1/2, y+1/2, z1/2; (vii) x, y, z1; (viii) x1/2, y+1/2, z+1/2; (ix) x+1/2, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H5···O2a0.9602.1013.044166.99
N1—H6···O3i0.9492.3663.157140.59
N2—H7···O3x0.9562.2803.163153.16
N2—H8···O2avii0.9582.4913.036116.01
N1a—H5a···O2iii0.9602.1013.044166.99
N1a—H6a···O3aii0.9492.3663.157140.59
N2a—H7a···O3aiv0.9562.2803.163153.16
N2a—H8a···O20.9582.4913.036116.01
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, z1; (x) x+1, y+1, z.
 
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