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catena-Poly[[[tetra­aqua­nickel(II)]-μ-4,4′-bipyridine-κ2N:N′] thio­sulfate dihydrate], {[Ni(C10H8N2)(H2O)4]S2O3·2H2O}n, (I), and catena-poly[[[tetra­aqua­nickel(II)]-μ-4,4′-bipyridine-κ2N:N′] sulfate methanol solvate monohydrate], {[Ni(C10H8N2)(H2O)4]SO4·CH4O·H2O}n, (II), are built up of {[Ni(4,4′-bipy)(H2O)4]2+}n chains (4,4′-bipy is 4,4′-bipyridine) inter­woven in an unusual P31 fashion. Voids are filled by the corresponding counter-anions and solvate mol­ecules, defining a complex three-dimensional network surrounding them. In both structures, the cationic chains evolve around a set of twofold axes passing through the NiII ions and bis­ecting the aromatic amines through their N (and their opposite C) atoms.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270107007214/av3057sup1.cif
Contains datablocks global, I, II

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270107007214/av3057Isup2.hkl
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270107007214/av3057IIsup3.hkl
Contains datablock II

CCDC references: 645513; 645514

Computing details top

For both compounds, data collection: SMART-NT (Bruker, 2001); cell refinement: SAINT-NT (Bruker, 2000); data reduction: SAINT-NT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-NT (Sheldrick, 2000); software used to prepare material for publication: SHELXTL-NT and PLATON (Spek, 2003).

(I) catena-Poly[[[tetraaquanickel(II)]-µ-4,4'-bipyridine-κ2N:N'] thiosulfate dihydrate] top
Crystal data top
[Ni(C10H8N2)(H2O)4]S2O3·2H2OF(000) = 678
Mr = 435.11Dx = 1.746 Mg m3
Hexagonal, P3121Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 31 2"µ = 1.47 mm1
a = 11.3363 (9) ÅT = 274 K
c = 11.1523 (13) ÅNeedles, colourless
V = 1241.2 (2) Å30.18 × 0.08 × 0.06 mm
Z = 3
Data collection top
Bruker SMART CCD area-detector
diffractometer
1907 independent reflections
Radiation source: fine-focus sealed tube1725 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.039
φ and ω scansθmax = 28.0°, θmin = 2.1°
Absorption correction: multi-scan
SADABS (Sheldrick, 2001)
h = 1414
Tmin = 0.78, Tmax = 0.92k = 1414
10484 measured reflectionsl = 1414
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)] = 0.035H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.082 w = 1/[σ2(Fo2) + (0.0412P)2 + 0.57P]
where P = (Fo2 + 2Fc2)/3
S = 0.98(Δ/σ)max = 0.004
1907 reflectionsΔρmax = 0.52 e Å3
153 parametersΔρmin = 0.31 e Å3
15 restraintsAbsolute structure: Flack (1983), with how many Friedel pairs?
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.02 (2)
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni11.00000.60675 (4)1.16670.02801 (14)
O1W1.1959 (2)0.6991 (2)1.1020 (2)0.0395 (5)
H1WB1.209 (4)0.649 (3)1.055 (3)0.066 (13)*
H1WA1.269 (2)0.742 (4)1.142 (3)0.058 (13)*
O2W1.0791 (2)0.6516 (2)1.33982 (19)0.0415 (5)
H2WB1.153 (2)0.726 (2)1.346 (3)0.067 (13)*
H2WA1.067 (3)0.613 (3)1.4072 (17)0.051 (11)*
O3W0.6763 (3)0.4299 (4)0.7414 (3)0.0827 (11)
H3WB0.649 (4)0.476 (4)0.781 (4)0.088 (18)*
H3WA0.756 (2)0.488 (4)0.719 (5)0.107 (19)*
N11.00000.7946 (3)1.16670.0312 (7)
N21.00001.4214 (3)1.16670.0319 (7)
C10.8852 (3)0.8001 (3)1.1688 (3)0.0430 (8)
H10.80310.71821.17010.052*
C20.8805 (3)0.9185 (3)1.1693 (3)0.0413 (7)
H20.79680.91501.17150.050*
C31.00001.0435 (3)1.16670.0322 (9)
C41.00001.1750 (4)1.16670.0342 (9)
C50.8901 (3)1.1831 (3)1.1244 (3)0.0406 (7)
H50.81381.10611.09480.049*
C60.8947 (3)1.3074 (3)1.1267 (3)0.0412 (7)
H60.81931.31101.09840.049*
S10.98833 (19)0.44014 (16)0.69163 (13)0.0388 (4)*0.50
S20.9882 (2)0.60284 (18)0.62674 (14)0.0477 (4)0.50
O10.9453 (7)0.4222 (6)0.8165 (4)0.078 (2)0.50
O21.1256 (9)0.4590 (16)0.6800 (11)0.078 (4)0.50
O30.8935 (9)0.3208 (9)0.6206 (8)0.044 (2)0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0303 (3)0.02351 (18)0.0325 (2)0.01516 (15)0.0027 (2)0.00133 (12)
O1W0.0394 (12)0.0334 (12)0.0460 (12)0.0184 (10)0.0053 (10)0.0006 (10)
O2W0.0447 (13)0.0362 (12)0.0329 (12)0.0123 (11)0.0058 (9)0.0011 (9)
O3W0.0427 (16)0.102 (3)0.0642 (19)0.0069 (18)0.0019 (14)0.0308 (19)
N10.039 (2)0.0268 (12)0.0322 (17)0.0193 (10)0.0010 (16)0.0005 (8)
N20.0353 (19)0.0257 (12)0.0380 (18)0.0177 (10)0.0083 (14)0.0042 (7)
C10.0390 (17)0.0300 (16)0.062 (2)0.0191 (13)0.0019 (14)0.0019 (14)
C20.0375 (17)0.0308 (16)0.059 (2)0.0195 (13)0.0029 (14)0.0010 (14)
C30.040 (2)0.0277 (15)0.033 (2)0.0199 (12)0.0058 (17)0.0029 (8)
C40.042 (2)0.0308 (16)0.033 (2)0.0211 (11)0.0058 (16)0.0029 (8)
C50.0377 (17)0.0273 (14)0.0577 (19)0.0169 (13)0.0173 (15)0.0110 (13)
C60.0418 (17)0.0331 (16)0.0556 (19)0.0239 (14)0.0163 (14)0.0087 (14)
S20.0513 (10)0.0433 (8)0.0521 (9)0.0263 (8)0.0103 (10)0.0113 (7)
O10.152 (7)0.053 (3)0.043 (3)0.062 (4)0.004 (3)0.001 (2)
O20.049 (5)0.069 (8)0.132 (11)0.041 (5)0.015 (6)0.016 (7)
O30.044 (3)0.042 (4)0.037 (3)0.016 (3)0.005 (2)0.001 (2)
Geometric parameters (Å, º) top
Ni1—O1Wi2.055 (2)N2—Ni1iii2.101 (3)
Ni1—O1W2.055 (2)C1—C21.370 (5)
Ni1—O2W2.082 (2)C1—H10.9300
Ni1—O2Wi2.082 (2)C2—C31.388 (4)
Ni1—N2ii2.101 (3)C2—H20.9300
Ni1—N12.129 (3)C3—C2i1.388 (4)
O1W—H1WA0.85 (4)C3—C41.490 (5)
O1W—H1WB0.85 (4)C4—C5i1.377 (4)
O2W—H2WA0.85 (2)C4—C51.377 (4)
O2W—H2WB0.85 (2)C5—C61.384 (4)
O3W—H3WA0.85 (5)C5—H50.9300
O3W—H3WB0.85 (5)C6—H60.9300
N1—C1i1.334 (4)S1—O11.456 (5)
N1—C11.334 (4)S1—O21.466 (6)
N2—C6i1.324 (4)S1—O31.470 (6)
N2—C61.324 (4)S1—S21.982 (2)
O1Wi—Ni1—O1W176.44 (13)C6i—N2—Ni1iii121.69 (19)
O2W—Ni1—O2Wi176.68 (14)C6—N2—Ni1iii121.69 (19)
N2ii—Ni1—N1180.000N1—C1—C2124.3 (3)
O1Wi—Ni1—O2W91.43 (9)N1—C1—H1117.9
O1W—Ni1—O2Wi91.42 (9)C2—C1—H1117.9
O1W—Ni1—O2W88.68 (9)C1—C2—C3120.3 (3)
O1Wi—Ni1—O2Wi88.68 (9)C1—C2—H2119.9
O1W—Ni1—N2ii88.22 (6)C3—C2—H2119.9
O1Wi—Ni1—N2ii88.22 (6)C2—C3—C2i115.5 (4)
O2W—Ni1—N2ii91.66 (7)C2—C3—C4122.2 (2)
O2Wi—Ni1—N2ii91.66 (7)C2i—C3—C4122.2 (2)
O1W—Ni1—N191.78 (6)C5i—C4—C5117.4 (4)
O1Wi—Ni1—N191.78 (6)C5i—C4—C3121.28 (19)
O2W—Ni1—N188.34 (7)C5—C4—C3121.28 (19)
O2Wi—Ni1—N188.34 (7)C4—C5—C6119.2 (3)
Ni1—O1W—H1WB113 (3)C4—C5—H5120.4
Ni1—O1W—H1WA127 (3)C6—C5—H5120.4
H1WB—O1W—H1WA106 (2)N2—C6—C5123.8 (3)
Ni1—O2W—H2WB115 (2)N2—C6—H6118.1
Ni1—O2W—H2WA139 (2)C5—C6—H6118.1
H2WB—O2W—H2WA105 (2)O1—S1—O2111.2 (5)
H3WB—O3W—H3WA104 (2)O1—S1—O3110.3 (4)
C1i—N1—C1115.4 (4)O2—S1—O3108.7 (4)
C1i—N1—Ni1122.31 (19)O1—S1—S2108.8 (2)
C1—N1—Ni1122.3 (2)O2—S1—S2109.0 (5)
C6i—N2—C6116.6 (4)O3—S1—S2108.6 (6)
Symmetry codes: (i) x+2, x+y+1, z+7/3; (ii) x, y1, z; (iii) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O1iv0.85 (4)2.13 (2)2.835 (7)140 (4)
O1W—H1WB···O3Wv0.85 (4)1.85 (2)2.681 (4)167 (4)
O2W—H2WA···O1i0.85 (2)1.91 (2)2.710 (5)156 (3)
O2W—H2WA···S2vi0.85 (2)2.59 (2)3.322 (3)146 (3)
O2W—H2WB···O2vii0.85 (2)1.88 (2)2.723 (7)169 (4)
O2W—H2WB···O3iv0.85 (2)1.93 (2)2.776 (7)174 (3)
O3W—H3WA···S20.85 (5)2.50 (2)3.324 (4)164 (4)
O3W—H3WA···S2viii0.85 (5)2.51 (2)3.322 (4)160 (5)
O3W—H3WB···O3ix0.85 (5)2.16 (2)2.862 (13)140 (5)
O3W—H3WB···O2x0.85 (5)2.39 (2)3.037 (14)134 (5)
O3W—H3WB···O1x0.85 (5)2.37 (2)3.196 (8)164 (5)
Symmetry codes: (i) x+2, x+y+1, z+7/3; (iv) y+1, x, z+2; (v) xy+1, y+1, z+5/3; (vi) x, y, z+1; (vii) x+y+2, x+2, z+2/3; (viii) x+2, x+y+1, z+4/3; (ix) y+1, xy, z+1/3; (x) xy, y+1, z+5/3.
(II) catena-poly[[[tetraaquanickel(II)]-µ-4,4'-bipyridine-κ2N:N'] sulfate methanol solvate monohydrate top
Crystal data top
[Ni(C10H8N2)(H2O)4]SO4·CH4O·H2ODx = 1.652 Mg m3
Mr = 433.08Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P3121Cell parameters from 2570 reflections
Hall symbol: P 31 2"θ = 2.3–21.6°
a = 11.2916 (10) ŵ = 1.29 mm1
c = 23.660 (3) ÅT = 273 K
V = 2612.5 (5) Å3Block, green
Z = 60.16 × 0.12 × 0.10 mm
F(000) = 1356
Data collection top
Bruker SMART CCD area-detector
diffractometer
3968 independent reflections
Radiation source: fine-focus sealed tube2906 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.076
φ and ω scansθmax = 28.4°, θmin = 2.1°
Absorption correction: multi-scan
SADABS (Sheldrick, 2001)
h = 147
Tmin = 0.82, Tmax = 0.88k = 014
21995 measured reflectionsl = 031
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)] = 0.068H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.144 w = 1/[σ2(Fo2) + (0.0429P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.92(Δ/σ)max = 0.017
3968 reflectionsΔρmax = 0.92 e Å3
265 parametersΔρmin = 0.49 e Å3
27 restraintsAbsolute structure: Flack (1983), with how many Friedel pairs?
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.01 (3)
Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.47361 (8)0.47361 (8)0.00000.0259 (2)
Ni21.00000.61953 (8)0.16670.0287 (3)
O1W0.5759 (4)0.3648 (4)0.01093 (17)0.0382 (10)
H1WA0.597 (6)0.341 (5)0.0203 (11)0.046*
H1WB0.559 (6)0.309 (5)0.0364 (15)0.046*
O2W0.4537 (4)0.4910 (4)0.08618 (15)0.0351 (9)
H2WA0.498 (5)0.469 (5)0.1086 (13)0.042*
H2WB0.459 (6)0.566 (4)0.0975 (14)0.042*
O3W1.1013 (4)0.6746 (5)0.09014 (16)0.0415 (10)
H3WA1.185 (2)0.702 (6)0.0928 (16)0.050*
H3WB1.061 (4)0.613 (4)0.0656 (14)0.050*
O4W0.8229 (4)0.5262 (4)0.12045 (16)0.0338 (9)
H4WA0.822 (4)0.470 (4)0.0978 (18)0.041*
H4WB0.750 (2)0.500 (5)0.1379 (16)0.041*
N10.2874 (6)0.2874 (6)0.00000.0303 (16)
N20.3394 (5)0.3394 (5)0.00000.0265 (14)
C10.2636 (6)0.1858 (6)0.0362 (2)0.0355 (14)
H10.33170.19990.06190.043*
C20.1443 (6)0.0629 (6)0.0370 (2)0.0327 (13)
H20.13340.00480.06230.039*
C30.0395 (7)0.0395 (7)0.00000.0273 (17)
C40.0910 (7)0.0910 (7)0.00000.0280 (18)
C50.0949 (6)0.2149 (6)0.0046 (3)0.0394 (15)
H50.01420.21750.00840.047*
C60.2181 (6)0.3336 (6)0.0037 (3)0.0371 (15)
H60.21780.41570.00580.045*
N31.00000.4318 (6)0.16670.0308 (16)
N41.00000.1937 (5)0.16670.0265 (15)
C70.8866 (6)0.3138 (6)0.1775 (3)0.0366 (14)
H70.80650.31510.18500.044*
C80.8827 (6)0.1901 (6)0.1782 (3)0.0373 (14)
H80.80140.11020.18640.045*
C91.00000.1848 (7)0.16670.0313 (18)
C101.00000.0532 (7)0.16670.0301 (19)
C110.8860 (6)0.0673 (6)0.1504 (2)0.0343 (14)
H110.80720.06790.13860.041*
C120.8910 (6)0.1869 (6)0.1518 (2)0.0344 (14)
H120.81260.26770.14180.041*
S10.47343 (15)0.81912 (15)0.11549 (6)0.0339 (3)
O10.5609 (5)0.9420 (4)0.08333 (18)0.0541 (13)
O20.3578 (5)0.7229 (5)0.07953 (18)0.0521 (13)
O30.5473 (5)0.7520 (5)0.1335 (2)0.0536 (12)
O40.4162 (5)0.8533 (5)0.16479 (18)0.0513 (13)
O1M0.4572 (6)0.9252 (6)0.0248 (2)0.0597 (14)
H1M0.500 (7)0.928 (8)0.005 (2)0.072*
C1M0.3325 (11)0.9186 (12)0.0222 (3)0.102 (4)
H1MA0.34601.00900.01730.153*
H1MB0.28120.86240.00920.153*
H1MC0.28300.87990.05660.153*
O5W0.5600 (8)1.1908 (6)0.0927 (2)0.0737 (18)
H5WA0.541 (9)1.215 (8)0.1242 (18)0.088*
H5WB0.569 (9)1.121 (6)0.099 (3)0.088*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0226 (4)0.0226 (4)0.0302 (5)0.0096 (4)0.0006 (2)0.0006 (2)
Ni20.0298 (6)0.0231 (4)0.0353 (6)0.0149 (3)0.0011 (4)0.0005 (2)
O1W0.044 (3)0.041 (3)0.038 (2)0.028 (2)0.008 (2)0.008 (2)
O2W0.041 (3)0.036 (2)0.030 (2)0.021 (2)0.0067 (18)0.0042 (17)
O3W0.041 (3)0.045 (3)0.042 (2)0.024 (2)0.004 (2)0.003 (2)
O4W0.034 (2)0.030 (2)0.041 (2)0.0182 (19)0.0034 (18)0.0089 (18)
N10.030 (3)0.030 (3)0.033 (4)0.016 (3)0.0024 (14)0.0024 (14)
N20.023 (2)0.023 (2)0.031 (3)0.009 (3)0.0037 (14)0.0037 (14)
C10.030 (3)0.035 (3)0.037 (3)0.013 (3)0.001 (2)0.003 (3)
C20.030 (3)0.031 (3)0.038 (3)0.016 (3)0.001 (3)0.007 (2)
C30.025 (3)0.025 (3)0.035 (4)0.014 (4)0.0019 (17)0.0019 (17)
C40.024 (3)0.024 (3)0.029 (4)0.007 (4)0.0009 (17)0.0009 (17)
C50.026 (3)0.033 (3)0.062 (4)0.017 (3)0.000 (3)0.000 (3)
C60.032 (3)0.025 (3)0.057 (4)0.015 (3)0.003 (3)0.000 (3)
N30.035 (4)0.022 (3)0.039 (4)0.018 (2)0.007 (3)0.0036 (16)
N40.026 (4)0.023 (2)0.032 (4)0.0128 (19)0.006 (3)0.0030 (13)
C70.029 (3)0.031 (3)0.055 (4)0.018 (3)0.005 (3)0.003 (3)
C80.033 (3)0.025 (3)0.055 (4)0.015 (3)0.005 (3)0.002 (3)
C90.037 (5)0.027 (3)0.034 (4)0.019 (2)0.002 (4)0.0012 (18)
C100.036 (5)0.031 (3)0.026 (4)0.018 (2)0.010 (3)0.0052 (17)
C110.035 (3)0.027 (3)0.045 (4)0.018 (3)0.001 (3)0.002 (3)
C120.036 (3)0.026 (3)0.041 (3)0.015 (3)0.001 (3)0.004 (3)
S10.0326 (8)0.0312 (8)0.0369 (8)0.0151 (6)0.0022 (6)0.0004 (6)
O10.054 (3)0.041 (3)0.063 (3)0.020 (2)0.022 (3)0.008 (2)
O20.047 (3)0.058 (3)0.050 (3)0.025 (2)0.009 (2)0.029 (2)
O30.048 (3)0.054 (3)0.064 (3)0.030 (3)0.001 (2)0.007 (2)
O40.043 (3)0.048 (3)0.043 (3)0.007 (2)0.007 (2)0.016 (2)
O1M0.080 (4)0.077 (4)0.048 (3)0.059 (3)0.014 (3)0.011 (3)
C1M0.132 (9)0.166 (12)0.059 (5)0.113 (9)0.031 (6)0.037 (6)
O5W0.137 (6)0.073 (4)0.046 (3)0.079 (4)0.019 (3)0.014 (3)
Geometric parameters (Å, º) top
Ni1—O2Wi2.072 (4)C4—C51.382 (7)
Ni1—O2W2.072 (4)C5—C61.367 (9)
Ni1—O1W2.081 (4)C5—H50.9300
Ni1—O1Wi2.081 (4)C6—H60.9300
Ni1—N12.103 (6)N3—C71.332 (6)
Ni1—N2ii2.112 (6)N3—C7iii1.332 (6)
Ni2—O4Wiii2.049 (4)N4—C12iii1.319 (7)
Ni2—O4W2.049 (4)N4—C121.319 (7)
Ni2—O3Wiii2.064 (4)C7—C81.376 (8)
Ni2—O3W2.064 (4)C7—H70.9300
Ni2—N4iv2.109 (6)C8—C91.383 (7)
Ni2—N32.120 (6)C8—H80.9300
O1W—H1WA0.86 (4)C9—C8iii1.383 (7)
O1W—H1WB0.82 (4)C9—C101.486 (11)
O2W—H2WA0.85 (4)C10—C11iii1.380 (7)
O2W—H2WB0.86 (4)C10—C111.380 (7)
O3W—H3WA0.83 (4)C11—C121.380 (8)
O3W—H3WB0.84 (4)C11—H110.9300
O4W—H4WA0.82 (4)C12—H120.9300
O4W—H4WB0.83 (4)S1—O31.444 (5)
N1—C1i1.347 (6)S1—O11.452 (4)
N1—C11.347 (6)S1—O41.475 (4)
N2—C61.341 (7)S1—O21.480 (4)
N2—C6i1.341 (6)O1M—C1M1.374 (10)
C1—C21.368 (7)O1M—H1M0.84 (5)
C1—H10.9300C1M—H1MA0.9600
C2—C31.387 (7)C1M—H1MB0.9600
C2—H20.9300C1M—H1MC0.9600
C3—C2i1.387 (7)O5W—H5WA0.86 (5)
C3—C41.474 (10)O5W—H5WB0.86 (5)
C4—C5i1.382 (7)
O2Wi—Ni1—O2W179.2 (2)C1—C2—H2120.1
O2Wi—Ni1—O1W86.98 (15)C3—C2—H2120.1
O2W—Ni1—O1W93.01 (15)C2—C3—C2i117.1 (7)
O2Wi—Ni1—O1Wi93.01 (15)C2—C3—C4121.4 (4)
O2W—Ni1—O1Wi86.98 (15)C2i—C3—C4121.4 (4)
O1W—Ni1—O1Wi178.0 (2)C5i—C4—C5117.1 (7)
O2Wi—Ni1—N189.61 (11)C5i—C4—C3121.4 (4)
O2W—Ni1—N189.61 (11)C5—C4—C3121.4 (4)
O1W—Ni1—N188.99 (12)C6—C5—C4119.5 (6)
O1Wi—Ni1—N188.99 (12)C6—C5—H5120.2
O2Wi—Ni1—N2ii90.39 (11)C4—C5—H5120.2
O2W—Ni1—N2ii90.39 (11)N2—C6—C5124.2 (6)
O1W—Ni1—N2ii91.01 (12)N2—C6—H6117.9
O1Wi—Ni1—N2ii91.01 (12)C5—C6—H6117.9
N1—Ni1—N2ii180.0C7—N3—C7iii117.4 (7)
O4Wiii—Ni2—O4W177.0 (2)C7—N3—Ni2121.3 (4)
O4Wiii—Ni2—O3Wiii86.45 (16)C7iii—N3—Ni2121.3 (4)
O4W—Ni2—O3Wiii93.63 (16)C12iii—N4—C12116.6 (7)
O4Wiii—Ni2—O3W93.63 (16)C12iii—N4—Ni2vi121.7 (4)
O4W—Ni2—O3W86.45 (16)C12—N4—Ni2vi121.7 (4)
O3Wiii—Ni2—O3W177.2 (2)N3—C7—C8123.0 (6)
O4Wiii—Ni2—N4iv91.51 (11)N3—C7—H7118.5
O4W—Ni2—N4iv91.51 (11)C8—C7—H7118.5
O3Wiii—Ni2—N4iv88.61 (12)C7—C8—C9119.7 (6)
O3W—Ni2—N4iv88.61 (12)C7—C8—H8120.1
O4Wiii—Ni2—N388.49 (11)C9—C8—H8120.1
O4W—Ni2—N388.49 (11)C8—C9—C8iii117.1 (8)
O3Wiii—Ni2—N391.39 (12)C8—C9—C10121.5 (4)
O3W—Ni2—N391.39 (12)C8iii—C9—C10121.5 (4)
N4iv—Ni2—N3180.000 (2)C11iii—C10—C11117.4 (8)
Ni1—O1W—H1WA114 (2)C11iii—C10—C9121.3 (4)
Ni1—O1W—H1WB124 (3)C11—C10—C9121.3 (4)
H1WA—O1W—H1WB112 (5)C12—C11—C10118.9 (6)
Ni1—O2W—H2WA118 (3)C12—C11—H11120.5
Ni1—O2W—H2WB116 (3)C10—C11—H11120.5
H2WA—O2W—H2WB109 (5)N4—C12—C11124.0 (6)
Ni2—O3W—H3WA114 (3)N4—C12—H12118.0
Ni2—O3W—H3WB111 (3)C11—C12—H12118.0
H3WA—O3W—H3WB114 (5)O3—S1—O1111.1 (3)
Ni2—O4W—H4WA112 (3)O3—S1—O4110.3 (3)
Ni2—O4W—H4WB117 (3)O1—S1—O4110.0 (3)
H4WA—O4W—H4WB115 (5)O3—S1—O2108.3 (3)
C1i—N1—C1116.6 (7)O1—S1—O2109.2 (3)
C1i—N1—Ni1121.7 (3)O4—S1—O2107.8 (3)
C1—N1—Ni1121.7 (3)C1M—O1M—H1M121 (6)
C6—N2—C6i115.3 (7)O1M—C1M—H1MA109.5
C6—N2—Ni1v122.3 (3)O1M—C1M—H1MB109.5
C6i—N2—Ni1v122.3 (3)H1MA—C1M—H1MB109.5
N1—C1—C2123.3 (6)O1M—C1M—H1MC109.5
N1—C1—H1118.4H1MA—C1M—H1MC109.5
C2—C1—H1118.4H1MB—C1M—H1MC109.5
C1—C2—C3119.9 (6)H5WA—O5W—H5WB108 (5)
Symmetry codes: (i) y, x, z; (ii) x+1, y+1, z; (iii) x+2, x+y+1, z+1/3; (iv) x, y+1, z; (v) x1, y1, z; (vi) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1WA···O2i0.86 (4)1.93 (4)2.734 (6)154 (6)
O1W—H1WB···O5Wvi0.82 (4)1.89 (4)2.699 (6)168 (5)
O2W—H2WA···O4vii0.85 (4)1.85 (4)2.687 (5)168 (4)
O2W—H2WB···O30.86 (4)2.01 (4)2.818 (6)156 (5)
O3W—H3WA···O2viii0.83 (4)1.87 (4)2.678 (6)161 (5)
O3W—H3WB···O1Mi0.84 (4)1.92 (4)2.736 (7)163 (4)
O4W—H4WA···O1Mi0.82 (4)2.13 (4)2.822 (6)141 (5)
O4W—H4WB···O4vii0.83 (4)1.79 (4)2.623 (6)174 (4)
O1M—H1M···O10.84 (5)1.96 (5)2.781 (7)164 (8)
O5W—H5WA···O3ix0.86 (5)2.02 (5)2.846 (7)161 (8)
O5W—H5WB···O10.86 (5)2.01 (5)2.823 (7)158 (7)
Symmetry codes: (i) y, x, z; (vi) x, y1, z; (vii) x+1, x+y, z+1/3; (viii) x+1, y, z; (ix) x+1, x+y+1, z+1/3.
 

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