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Initial attempts to make [Ni(H2O)2(15-crown-5)](NO3)2, i.e. to insert the Ni2+ ion into the 15-crown-5 macrocycle, gave the mono- (two polymorphs) and dihydrate of a co-crystal of [Ni(H2O)6](NO3)2 and 15-crown-5 (1,4,7,10,13-pentaoxacyclopentadecane = 15C5). Synthetic routes designed to restrict the water available to the Ni2+ cation gave three additional compounds, [Ni(H2O)6](NO3)2-trans-[Ni(H2O)4(MeOH)2](NO3)2·2(15C5), cis-[Ni(H2O)4(NO3)2]-trans-[Ni(H2O)4(NO3)2]·2(15C5) and [Ni(H2O)2(MeCN)(NO3)2]·15C5·MeCN. All five compounds contain Ni2+ ions with two trans aqua ligands. In all six structures these aqua ligands make hydrogen bonds to the 15C5 molecules to form stacks in which the Ni complexes and 15C5 molecules alternate. The structures are surprisingly complicated: all are co-crystals, some are also solvates, and most have Z′ > 1. The target compound was finally prepared by heating pale green crystals of [Ni(H2O)6](NO3)2·15C5·2H2O to over 350 K and then cooling the resulting mixture of yellow crystals and solution to room temperature. Formation of the target compound seems to be favored at higher temperatures by a positive ΔrxnSo and an increased rate of ligand exchange.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768108034058/bs5068sup1.cif
Contains datablocks 1, 2a, 2b, 3, 4, 5, 6

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108034058/bs50681sup2.hkl
Contains datablock 1

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108034058/bs50682asup3.hkl
Contains datablock 2a

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108034058/bs50682bsup4.hkl
Contains datablock 2b

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108034058/bs50683sup5.hkl
Contains datablock 3

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108034058/bs50684sup6.hkl
Contains datablock 4

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108034058/bs50685sup7.hkl
Contains datablock 5

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768108034058/bs50686sup8.hkl
Contains datablock 6

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108768108034058/bs5068sup9.pdf
Extra figures, including DSC traces and ellisoid plots

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108768108034058/bs5068sup10.pdf
Crystal images through microscope during heating

CCDC references: 718168; 718169; 718170; 718171; 718172; 718173; 718174

Computing details top

For all compounds, data collection: COLLECT (Nonius, 1999); cell refinement: DENZO-SMN (Otwinowski & Minor, 2006); data reduction: DENZO-SMN (Otwinowski & Minor, 2006); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008). Molecular graphics: XP in SHELXTL (Mercury (Macrae et al., 2008)8) for (1); XP in SHELXTL (Mercury (Macrae et al., 2008) for (2a), (2b), (3), (4), (5); XP in Siemens SHELXTL (Sheldrick, 2008), Mercury (Macrae et al., 2006) for (6). For all compounds, software used to prepare material for publication: SHELX97 and local procedures.

(1) top
Crystal data top
C10H20O5·H12NiO62+·2(NO3)·2(H2O)F(000) = 1160
Mr = 547.12Dx = 1.530 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5679 reflections
a = 11.950 (1) Åθ = 1.0–27.5°
b = 12.686 (1) ŵ = 0.90 mm1
c = 15.988 (1) ÅT = 90 K
β = 101.51 (1)°Parallelepiped, pale green
V = 2375.0 (3) Å30.30 × 0.25 × 0.20 mm
Z = 4
Data collection top
Nonius KappaCCD
diffractometer
5463 independent reflections
Radiation source: fine-focus sealed tube3979 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
Detector resolution: 18 pixels mm-1θmax = 27.5°, θmin = 1.7°
ω scans at fixed χ = 55°h = 1515
Absorption correction: multi-scan
Scalepack (Otwinowski & Minor, 2006)
k = 1616
Tmin = 0.773, Tmax = 0.840l = 2020
10666 measured reflections
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)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.109H atoms treated by a mixture of independent and constrained refinement
S = 1.06 w = 1/[σ2(Fo2) + (0.0591P)2 + 0.0953P]
where P = (Fo2 + 2Fc2)/3
5463 reflections(Δ/σ)max < 0.001
338 parametersΔρmax = 0.86 e Å3
24 restraintsΔρmin = 0.53 e Å3
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.03958 (19)0.14224 (17)0.33492 (15)0.0211 (5)
H1A0.04070.14420.27320.025*
H1B0.03850.12320.34170.025*
C20.1241 (2)0.06217 (18)0.37905 (15)0.0230 (5)
H2A0.12460.06150.44100.028*
H2B0.10300.00910.35590.028*
C30.3242 (2)0.02237 (17)0.40505 (15)0.0235 (6)
H3A0.32390.04310.37130.028*
H3B0.31280.00300.46280.028*
C40.43581 (19)0.07826 (18)0.41146 (15)0.0224 (5)
H4A0.49940.02690.42290.027*
H4B0.43810.11480.35710.027*
C50.5425 (2)0.22511 (19)0.48578 (16)0.0236 (6)
H5A0.60880.18650.47250.028*
H5B0.56400.25160.54510.028*
C60.51558 (19)0.31702 (18)0.42609 (16)0.0220 (5)
H6A0.58230.36470.43280.026*
H6B0.49780.29180.36630.026*
C70.39404 (19)0.46548 (17)0.39577 (15)0.0203 (5)
H7A0.40270.45230.33640.024*
H7B0.44730.52260.41980.024*
C80.27326 (18)0.49780 (17)0.39676 (14)0.0203 (5)
H8A0.26090.50070.45610.024*
H8B0.25720.56830.37060.024*
C90.08363 (18)0.42862 (18)0.35669 (15)0.0202 (5)
H9A0.04760.49100.32510.024*
H9B0.07840.43610.41740.024*
C100.02372 (19)0.32935 (18)0.31987 (15)0.0208 (5)
H10A0.05930.33500.31840.025*
H10B0.03520.31840.26080.025*
O10.07067 (13)0.24319 (11)0.37265 (10)0.0184 (4)
O20.23410 (12)0.09047 (12)0.36458 (10)0.0204 (4)
O30.44751 (13)0.15343 (12)0.47989 (10)0.0200 (4)
O40.41993 (12)0.37208 (12)0.44538 (10)0.0184 (4)
O50.20055 (13)0.42081 (12)0.34906 (10)0.0180 (4)
Ni0.25925 (2)0.24027 (2)0.140934 (18)0.01200 (10)
O60.28631 (13)0.25744 (11)0.27029 (10)0.0145 (3)
H6C0.2519 (17)0.3101 (9)0.2837 (14)0.022*
H6D0.2639 (18)0.2072 (10)0.2968 (14)0.022*
O70.24109 (13)0.21594 (13)0.01288 (10)0.0190 (4)
H7C0.1933 (14)0.2402 (17)0.0286 (11)0.028*
H7D0.2997 (12)0.2056 (18)0.0066 (14)0.028*
O80.13210 (12)0.13215 (12)0.14530 (10)0.0161 (3)
H8C0.1500 (17)0.0687 (9)0.1505 (14)0.024*
H8D0.0747 (14)0.1356 (16)0.1059 (11)0.024*
O90.37998 (13)0.12260 (12)0.15538 (10)0.0178 (3)
H9C0.3583 (16)0.0608 (9)0.1558 (15)0.027*
H9D0.4448 (11)0.1264 (16)0.1864 (13)0.027*
O100.38594 (12)0.34916 (12)0.13966 (10)0.0163 (3)
H10C0.3934 (17)0.3558 (19)0.0896 (6)0.024*
H10D0.4506 (11)0.3314 (18)0.1678 (11)0.024*
O110.14051 (12)0.35750 (12)0.12589 (10)0.0170 (3)
H11C0.1639 (16)0.4162 (11)0.1126 (14)0.025*
H11D0.0792 (12)0.3484 (17)0.0907 (12)0.025*
N10.65678 (17)0.22118 (16)0.24141 (13)0.0214 (5)
O120.59872 (13)0.14155 (13)0.25296 (11)0.0268 (4)
O130.76169 (14)0.21516 (14)0.25024 (13)0.0357 (5)
O140.60726 (13)0.30809 (12)0.22190 (11)0.0248 (4)
N20.10946 (17)0.22812 (15)0.00317 (13)0.0204 (4)
O150.05771 (13)0.14346 (12)0.01778 (10)0.0234 (4)
O160.20209 (14)0.22689 (13)0.05639 (12)0.0300 (4)
O170.07137 (13)0.31451 (12)0.02775 (11)0.0280 (4)
O180.23536 (16)0.54416 (13)0.09808 (12)0.0295 (4)
H18C0.262 (2)0.5620 (19)0.1493 (7)0.044*
H18D0.205 (2)0.5999 (13)0.0751 (13)0.044*
O190.25170 (14)0.05515 (12)0.16160 (12)0.0244 (4)
H19C0.240 (2)0.0924 (16)0.1178 (8)0.037*
H19D0.276 (2)0.0945 (15)0.2029 (9)0.037*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.0227 (13)0.0225 (13)0.0198 (13)0.0093 (10)0.0086 (10)0.0071 (10)
C20.0311 (14)0.0183 (12)0.0222 (14)0.0062 (10)0.0114 (11)0.0010 (10)
C30.0372 (15)0.0149 (12)0.0184 (13)0.0082 (10)0.0053 (11)0.0013 (10)
C40.0276 (14)0.0237 (13)0.0174 (13)0.0134 (10)0.0083 (11)0.0036 (10)
C50.0131 (12)0.0334 (14)0.0245 (14)0.0005 (10)0.0042 (10)0.0040 (11)
C60.0182 (12)0.0247 (13)0.0249 (14)0.0014 (10)0.0087 (10)0.0020 (10)
C70.0256 (13)0.0175 (12)0.0185 (13)0.0064 (10)0.0063 (10)0.0002 (10)
C80.0293 (14)0.0125 (11)0.0196 (13)0.0029 (10)0.0060 (11)0.0026 (9)
C90.0187 (13)0.0204 (12)0.0234 (13)0.0065 (10)0.0089 (10)0.0015 (10)
C100.0174 (12)0.0263 (13)0.0185 (13)0.0053 (10)0.0035 (10)0.0039 (10)
O10.0198 (9)0.0190 (9)0.0156 (9)0.0013 (6)0.0016 (7)0.0016 (6)
O20.0226 (9)0.0184 (9)0.0210 (9)0.0014 (7)0.0060 (7)0.0076 (7)
O30.0225 (9)0.0186 (8)0.0213 (9)0.0031 (7)0.0098 (7)0.0014 (7)
O40.0164 (8)0.0192 (8)0.0215 (9)0.0007 (6)0.0086 (7)0.0011 (7)
O50.0191 (8)0.0165 (8)0.0200 (9)0.0008 (6)0.0077 (7)0.0029 (7)
Ni0.01211 (17)0.01298 (16)0.01132 (17)0.00002 (11)0.00331 (11)0.00008 (11)
O60.0166 (9)0.0154 (8)0.0119 (8)0.0015 (6)0.0039 (6)0.0002 (6)
O70.0132 (9)0.0327 (9)0.0113 (9)0.0015 (7)0.0029 (7)0.0005 (7)
O80.0141 (8)0.0130 (8)0.0198 (9)0.0008 (6)0.0001 (6)0.0023 (7)
O90.0129 (8)0.0141 (8)0.0251 (10)0.0018 (6)0.0003 (7)0.0019 (7)
O100.0146 (8)0.0176 (8)0.0165 (9)0.0027 (6)0.0027 (7)0.0039 (7)
O110.0147 (8)0.0136 (8)0.0220 (9)0.0001 (6)0.0021 (7)0.0012 (7)
N10.0204 (12)0.0247 (11)0.0197 (11)0.0001 (8)0.0050 (9)0.0032 (9)
O120.0234 (9)0.0191 (9)0.0357 (11)0.0046 (7)0.0010 (8)0.0022 (8)
O130.0154 (10)0.0388 (11)0.0521 (13)0.0001 (8)0.0045 (9)0.0090 (9)
O140.0221 (9)0.0218 (9)0.0279 (10)0.0007 (7)0.0014 (7)0.0068 (7)
N20.0161 (11)0.0255 (11)0.0206 (11)0.0017 (8)0.0060 (9)0.0002 (9)
O150.0214 (9)0.0205 (9)0.0265 (10)0.0037 (7)0.0000 (7)0.0067 (7)
O160.0182 (10)0.0342 (10)0.0316 (11)0.0081 (7)0.0091 (8)0.0072 (8)
O170.0234 (9)0.0208 (9)0.0376 (11)0.0001 (7)0.0005 (8)0.0069 (8)
O180.0391 (12)0.0160 (9)0.0347 (11)0.0025 (8)0.0109 (9)0.0031 (8)
O190.0244 (10)0.0147 (9)0.0327 (11)0.0003 (7)0.0026 (8)0.0007 (7)
Geometric parameters (Å, º) top
C1—O11.433 (3)C10—O11.426 (3)
C1—C21.505 (3)C10—H10A0.9900
C1—H1A0.9900C10—H10B0.9900
C1—H1B0.9900Ni—O112.0363 (15)
C2—O21.425 (3)Ni—O72.0387 (15)
C2—H2A0.9900Ni—O62.0402 (16)
C2—H2B0.9900Ni—O102.0525 (15)
C3—O21.430 (3)Ni—O92.0566 (14)
C3—C41.496 (3)Ni—O82.0584 (15)
C3—H3A0.9900O6—H6C0.835 (9)
C3—H3B0.9900O6—H6D0.839 (9)
C4—O31.437 (3)O7—H7C0.842 (9)
C4—H4A0.9900O7—H7D0.832 (9)
C4—H4B0.9900O8—H8C0.833 (9)
C5—O31.442 (3)O8—H8D0.835 (9)
C5—C61.500 (3)O9—H9C0.826 (9)
C5—H5A0.9900O9—H9D0.833 (9)
C5—H5B0.9900O10—H10C0.826 (9)
C6—O41.425 (3)O10—H10D0.844 (9)
C6—H6A0.9900O11—H11C0.837 (9)
C6—H6B0.9900O11—H11D0.837 (9)
C7—O41.425 (3)N1—O131.236 (2)
C7—C81.504 (3)N1—O121.260 (2)
C7—H7A0.9900N1—O141.261 (2)
C7—H7B0.9900N2—O171.250 (2)
C8—O51.423 (3)N2—O151.251 (2)
C8—H8A0.9900N2—O161.254 (3)
C8—H8B0.9900O18—H18C0.849 (9)
C9—O51.430 (2)O18—H18D0.842 (9)
C9—C101.509 (3)O19—H19C0.834 (9)
C9—H9A0.9900O19—H19D0.832 (9)
C9—H9B0.9900
O1—C1—C2108.20 (18)H9A—C9—H9B108.5
O1—C1—H1A110.1O1—C10—C9107.99 (18)
C2—C1—H1A110.1O1—C10—H10A110.1
O1—C1—H1B110.1C9—C10—H10A110.1
C2—C1—H1B110.1O1—C10—H10B110.1
H1A—C1—H1B108.4C9—C10—H10B110.1
O2—C2—C1107.96 (17)H10A—C10—H10B108.4
O2—C2—H2A110.1C10—O1—C1113.44 (18)
C1—C2—H2A110.1C2—O2—C3114.18 (17)
O2—C2—H2B110.1C4—O3—C5115.08 (16)
C1—C2—H2B110.1C6—O4—C7112.43 (16)
H2A—C2—H2B108.4C8—O5—C9114.15 (16)
O2—C3—C4108.96 (18)O11—Ni—O793.43 (7)
O2—C3—H3A109.9O11—Ni—O690.43 (6)
C4—C3—H3A109.9O7—Ni—O6176.12 (6)
O2—C3—H3B109.9O11—Ni—O1090.30 (6)
C4—C3—H3B109.9O7—Ni—O1091.31 (6)
H3A—C3—H3B108.3O6—Ni—O1088.29 (6)
O3—C4—C3108.46 (17)O11—Ni—O9179.47 (6)
O3—C4—H4A110.0O7—Ni—O986.25 (7)
C3—C4—H4A110.0O6—Ni—O989.88 (6)
O3—C4—H4B110.0O10—Ni—O989.27 (6)
C3—C4—H4B110.0O11—Ni—O889.37 (6)
H4A—C4—H4B108.4O7—Ni—O890.10 (6)
O3—C5—C6112.50 (19)O6—Ni—O890.32 (6)
O3—C5—H5A109.1O10—Ni—O8178.57 (6)
C6—C5—H5A109.1O9—Ni—O891.07 (6)
O3—C5—H5B109.1Ni—O6—H6C111.0 (16)
C6—C5—H5B109.1Ni—O6—H6D115.4 (16)
H5A—C5—H5B107.8H6C—O6—H6D104.8 (14)
O4—C6—C5108.81 (18)Ni—O7—H7C130.9 (16)
O4—C6—H6A109.9Ni—O7—H7D118.1 (16)
C5—C6—H6A109.9H7C—O7—H7D104.6 (14)
O4—C6—H6B109.9Ni—O8—H8C118.1 (15)
C5—C6—H6B109.9Ni—O8—H8D116.1 (16)
H6A—C6—H6B108.3H8C—O8—H8D106.4 (14)
O4—C7—C8108.85 (17)Ni—O9—H9C118.4 (15)
O4—C7—H7A109.9Ni—O9—H9D124.9 (15)
C8—C7—H7A109.9H9C—O9—H9D107.9 (14)
O4—C7—H7B109.9Ni—O10—H10C107.5 (16)
C8—C7—H7B109.9Ni—O10—H10D114.5 (16)
H7A—C7—H7B108.3H10C—O10—H10D106.2 (13)
O5—C8—C7106.97 (17)Ni—O11—H11C114.8 (15)
O5—C8—H8A110.3Ni—O11—H11D118.3 (16)
C7—C8—H8A110.3H11C—O11—H11D104.1 (14)
O5—C8—H8B110.3O13—N1—O12120.6 (2)
C7—C8—H8B110.3O13—N1—O14119.9 (2)
H8A—C8—H8B108.6O12—N1—O14119.50 (19)
O5—C9—C10107.73 (17)O17—N2—O15121.7 (2)
O5—C9—H9A110.2O17—N2—O16118.78 (19)
C10—C9—H9A110.2O15—N2—O16119.54 (19)
O5—C9—H9B110.2H18C—O18—H18D104.1 (14)
C10—C9—H9B110.2H19C—O19—H19D107.5 (15)
O1—C1—C2—O262.1 (2)C4—C3—O2—C2160.60 (18)
O2—C3—C4—O376.5 (2)C3—C4—O3—C5170.80 (18)
O3—C5—C6—O458.7 (3)C6—C5—O3—C482.7 (2)
O4—C7—C8—O568.9 (2)C5—C6—O4—C7175.50 (19)
O5—C9—C10—O165.7 (2)C8—C7—O4—C6160.76 (18)
C9—C10—O1—C1167.05 (17)C7—C8—O5—C9168.99 (17)
C2—C1—O1—C10159.91 (17)C10—C9—O5—C8167.49 (18)
C1—C2—O2—C3178.40 (18)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6—H6D···O20.84 (1)1.91 (1)2.743 (2)172 (2)
O6—H6C···O50.84 (1)1.92 (1)2.729 (2)162 (2)
O7—H7C···O1i0.84 (1)1.94 (1)2.761 (2)165 (2)
O7—H7D···O3i0.83 (1)2.55 (2)3.103 (2)125 (2)
O7—H7D···O4i0.83 (1)2.02 (1)2.811 (2)160 (2)
O8—H8D···O150.84 (1)1.90 (1)2.734 (2)179 (2)
O8—H8C···O190.83 (1)1.97 (1)2.758 (2)157 (2)
O9—H9D···O120.83 (1)1.94 (1)2.774 (2)176 (2)
O9—H9C···O190.83 (1)1.96 (1)2.740 (2)157 (2)
O10—H10C···O3i0.83 (1)1.99 (1)2.796 (2)164 (2)
O10—H10D···O140.84 (1)1.92 (1)2.758 (2)171 (2)
O11—H11D···O170.84 (1)1.93 (1)2.754 (2)169 (2)
O11—H11C···O180.84 (1)1.87 (1)2.700 (2)171 (2)
O18—H18C···O12ii0.85 (1)2.28 (2)3.041 (2)150 (2)
O18—H18C···O13ii0.85 (1)2.57 (2)3.249 (3)137 (2)
O18—H18D···O16iii0.84 (1)2.22 (2)2.989 (2)152 (2)
O18—H18D···O17iii0.84 (1)2.32 (1)3.087 (2)151 (2)
O19—H19D···O13iv0.83 (1)2.59 (2)3.255 (2)137 (2)
O19—H19D···O14iv0.83 (1)2.06 (1)2.840 (2)155 (2)
O19—H19C···O16v0.83 (1)1.98 (2)2.744 (2)153 (2)
Symmetry codes: (i) x, y+1/2, z1/2; (ii) x+1, y+1/2, z+1/2; (iii) x, y+1, z; (iv) x+1, y1/2, z+1/2; (v) x, y, z.
(2a) top
Crystal data top
C10H20O5·H12NiO62+·2(NO3)·H2OF(000) = 2240
Mr = 529.10Dx = 1.535 Mg m3
Monoclinic, B21Mo Kα radiation, λ = 0.71073 Å
a = 16.176 (2) ÅCell parameters from 5425 reflections
b = 16.514 (2) Åθ = 1.0–27.5°
c = 17.876 (2) ŵ = 0.93 mm1
β = 106.42 (1)°T = 90 K
V = 4580.5 (10) Å3Parallelepiped, pale green
Z = 80.40 × 0.20 × 0.20 mm
Data collection top
Nonius KappaCCD
diffractometer
10301 independent reflections
Radiation source: fine-focus sealed tube8534 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.000
Detector resolution: 18 pixels mm-1θmax = 27.5°, θmin = 1.5°
ω scans at fixed χ = 55°h = 2020
Absorption correction: multi-scan
Scalepack (Otwinowski & Minor, 2006)
k = 2120
Tmin = 0.707, Tmax = 0.836l = 2323
10301 measured reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH atoms treated by a mixture of independent and constrained refinement
R[F2 > 2σ(F2)] = 0.031 w = 1/[σ2(Fo2) + (0.0249P)2 + 2.8514P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.069(Δ/σ)max = 0.002
S = 1.04Δρmax = 0.58 e Å3
10301 reflectionsΔρmin = 0.41 e Å3
648 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
43 restraintsExtinction coefficient: 0.00036 (6)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack H D (1983), Acta Cryst. A39, 876-881
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.002 (7)
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C1_10.04439 (17)0.18343 (16)0.05096 (13)0.0231 (6)
H1A_10.00510.14090.02180.028*
H1B_10.10410.16890.05210.028*
C2_10.02062 (15)0.26447 (16)0.01186 (14)0.0215 (6)
H2A_10.00740.25810.04540.026*
H2B_10.03140.28590.02380.026*
C3_10.06835 (16)0.40306 (16)0.01996 (13)0.0229 (6)
H3A_10.02860.40600.03350.027*
H3B_10.12110.43380.02050.027*
C4_10.02621 (15)0.44161 (16)0.07578 (14)0.0218 (5)
H4A_10.01330.49920.06180.026*
H4B_10.02850.41360.07350.026*
C5_10.05249 (16)0.47752 (16)0.20859 (14)0.0192 (6)
H5A_10.00960.46600.19970.023*
H5B_10.05960.53660.20360.023*
C6_10.10217 (15)0.44992 (15)0.28862 (14)0.0203 (5)
H6A_10.16480.45160.29410.024*
H6B_10.09020.48600.32850.024*
C7_10.13483 (15)0.32544 (15)0.36078 (13)0.0192 (6)
H7A_10.13420.34820.41180.023*
H7B_10.19410.33000.35590.023*
C8_10.10753 (16)0.23881 (16)0.35541 (14)0.0207 (5)
H8A_10.14280.20840.40110.025*
H8B_10.04630.23480.35500.025*
C9_10.06617 (16)0.13652 (15)0.25657 (14)0.0202 (6)
H9A_10.00590.14740.25620.024*
H9B_10.08730.08910.29040.024*
C10_10.07072 (16)0.12003 (16)0.17554 (15)0.0235 (6)
H10A_10.13120.11010.17590.028*
H10B_10.03630.07140.15430.028*
O1_10.03728 (10)0.18919 (10)0.12830 (9)0.0189 (4)
O2_10.09079 (10)0.32002 (11)0.03908 (9)0.0202 (4)
O3_10.08397 (10)0.43561 (10)0.15234 (9)0.0184 (4)
O4_10.07606 (10)0.36869 (10)0.29909 (9)0.0185 (4)
O5_10.11873 (10)0.20532 (10)0.28515 (9)0.0184 (4)
Ni1_10.325421 (16)0.301237 (17)0.198968 (14)0.00986 (7)
O6_10.20285 (9)0.30515 (12)0.20931 (9)0.0155 (3)
H6C_10.1676 (12)0.3409 (10)0.1890 (14)0.023*
H6D_10.1747 (13)0.2715 (11)0.2273 (14)0.023*
O7_10.44503 (9)0.30994 (10)0.18265 (8)0.0130 (3)
H7C_10.4853 (11)0.3179 (14)0.2228 (8)0.020*
H7D_10.4651 (13)0.2767 (12)0.1568 (11)0.020*
O8_10.27377 (10)0.32585 (10)0.08305 (9)0.0161 (3)
H8C_10.2209 (6)0.3210 (14)0.0650 (13)0.024*
H8D_10.2882 (13)0.3606 (13)0.0548 (12)0.024*
O9_10.34170 (10)0.42168 (9)0.23208 (9)0.0153 (3)
H9C_10.3136 (14)0.4515 (13)0.1966 (9)0.023*
H9D_10.3282 (15)0.4371 (15)0.2719 (8)0.023*
O10_10.37385 (10)0.26884 (10)0.31447 (8)0.0140 (3)
H10C_10.3700 (15)0.3042 (9)0.3478 (11)0.021*
H10D_10.3584 (16)0.2261 (8)0.3337 (13)0.021*
O11_10.32119 (10)0.18011 (10)0.17230 (9)0.0159 (3)
H11C_10.2959 (15)0.1557 (14)0.1999 (10)0.024*
H11D_10.3012 (15)0.1617 (14)0.1273 (7)0.024*
N1_10.32437 (11)0.43406 (12)0.43286 (10)0.0143 (4)
O12_10.35105 (11)0.36294 (10)0.43343 (9)0.0211 (4)
O13_10.30140 (11)0.45917 (10)0.49027 (9)0.0213 (4)
O14_10.31961 (12)0.47919 (11)0.37612 (10)0.0239 (4)
N2_10.28287 (13)0.08032 (12)0.34666 (11)0.0187 (4)
O15_10.27197 (10)0.07636 (10)0.27462 (8)0.0174 (4)
O16_10.24559 (11)0.03107 (10)0.37932 (9)0.0237 (4)
O17_10.33073 (13)0.13364 (11)0.38673 (10)0.0310 (5)
O18_10.2562 (3)0.1252 (2)0.02488 (16)0.0294 (9)0.809 (9)
O18'_10.2987 (12)0.1052 (9)0.0363 (8)0.0294 (9)0.191 (9)
H18C_10.2860 (19)0.1292 (16)0.0066 (16)0.044*
H18D_10.2439 (19)0.0758 (8)0.0235 (17)0.044*
C1_20.53107 (16)0.22805 (16)0.02330 (13)0.0214 (5)
H1A_20.48680.19610.01490.026*
H1B_20.58840.21270.01830.026*
C2_20.51571 (14)0.31704 (15)0.00768 (13)0.0178 (5)
H2A_20.49930.32720.04920.021*
H2B_20.46800.33560.02800.021*
C3_20.57909 (16)0.44617 (15)0.04688 (14)0.0230 (6)
H3A_20.53920.46360.00340.028*
H3B_20.63470.47440.05350.028*
C4_20.54211 (16)0.47005 (16)0.11259 (14)0.0226 (6)
H4A_20.53730.52970.11490.027*
H4B_20.48390.44640.10400.027*
C5_20.57666 (16)0.46905 (16)0.25100 (14)0.0203 (6)
H5A_20.51360.46530.24260.024*
H5B_20.59390.52650.26080.024*
C6_20.62248 (15)0.41848 (15)0.31943 (13)0.0211 (5)
H6A_20.68370.41190.32080.025*
H6B_20.62010.44500.36840.025*
C7_20.63007 (15)0.27862 (16)0.36054 (13)0.0200 (6)
H7A_20.62960.28660.41530.024*
H7B_20.69060.27990.35860.024*
C8_20.58956 (16)0.19899 (16)0.33080 (13)0.0199 (5)
H8A_20.61570.15490.36740.024*
H8B_20.52690.20040.32500.024*
C9_20.55234 (16)0.12473 (15)0.20976 (14)0.0177 (5)
H9A_20.49170.13120.21040.021*
H9B_20.57250.07040.23040.021*
C10_20.55897 (16)0.13350 (15)0.12790 (14)0.0189 (5)
H10A_20.61970.12810.12730.023*
H10B_20.52450.09100.09400.023*
O1_20.52681 (10)0.21182 (10)0.10056 (9)0.0181 (4)
O2_20.59253 (10)0.36047 (11)0.04492 (9)0.0193 (4)
O3_20.59857 (10)0.44038 (10)0.18339 (9)0.0185 (4)
O4_20.58130 (10)0.34137 (10)0.31210 (9)0.0181 (4)
O5_20.60505 (10)0.18609 (10)0.25677 (9)0.0170 (3)
Ni2_20.825118 (16)0.297252 (17)0.196959 (14)0.00979 (7)
O6_20.70295 (9)0.30002 (12)0.20898 (9)0.0145 (3)
H6C_20.6706 (13)0.3395 (9)0.1940 (14)0.022*
H6D_20.6730 (13)0.2655 (10)0.2225 (14)0.022*
O7_20.94396 (9)0.30420 (11)0.17956 (8)0.0124 (3)
H7C_20.9844 (11)0.3188 (13)0.2183 (9)0.019*
H7D_20.9673 (13)0.2658 (11)0.1615 (12)0.019*
O8_20.77091 (10)0.32865 (10)0.08252 (9)0.0150 (3)
H8C_20.7180 (6)0.3368 (14)0.0701 (14)0.022*
H8D_20.7905 (12)0.3657 (12)0.0605 (13)0.022*
O9_20.84586 (10)0.41468 (9)0.23555 (9)0.0149 (3)
H9C_20.8200 (15)0.4487 (12)0.2029 (9)0.022*
H9D_20.8410 (15)0.4301 (14)0.2783 (7)0.022*
O10_20.87546 (10)0.26236 (10)0.31186 (9)0.0139 (3)
H10C_20.8635 (15)0.2965 (10)0.3426 (12)0.021*
H10D_20.8569 (15)0.2187 (8)0.3254 (13)0.021*
O11_20.81789 (10)0.17723 (10)0.16744 (9)0.0153 (3)
H11C_20.7946 (15)0.1490 (14)0.1951 (10)0.023*
H11D_20.7942 (14)0.1609 (14)0.1218 (6)0.023*
N1_20.83228 (12)0.42409 (12)0.43458 (10)0.0163 (4)
O12_20.82528 (10)0.34915 (10)0.42234 (9)0.0182 (4)
O13_20.81966 (12)0.45213 (10)0.49524 (9)0.0235 (4)
O14_20.85093 (13)0.46915 (11)0.38624 (10)0.0319 (5)
N2_20.76602 (12)0.08139 (11)0.33450 (11)0.0163 (4)
O15_20.75992 (10)0.07435 (9)0.26371 (9)0.0182 (4)
O16_20.72429 (11)0.03497 (10)0.36583 (9)0.0204 (4)
O17_20.81366 (12)0.13438 (11)0.37563 (10)0.0270 (4)
O18_20.74373 (15)0.11927 (12)0.02295 (11)0.0358 (5)
H18C_20.7836 (16)0.1172 (17)0.0001 (19)0.054*
H18D_20.7251 (18)0.0712 (9)0.0173 (18)0.054*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C1_10.0232 (14)0.0287 (14)0.0172 (12)0.0007 (11)0.0056 (10)0.0094 (11)
C2_10.0157 (13)0.0340 (15)0.0140 (12)0.0001 (11)0.0031 (10)0.0031 (11)
C3_10.0215 (13)0.0300 (15)0.0167 (12)0.0029 (11)0.0047 (10)0.0074 (11)
C4_10.0178 (13)0.0233 (13)0.0231 (13)0.0061 (11)0.0039 (10)0.0052 (11)
C5_10.0182 (13)0.0158 (13)0.0261 (14)0.0006 (11)0.0102 (11)0.0057 (11)
C6_10.0176 (12)0.0216 (13)0.0236 (13)0.0069 (10)0.0088 (10)0.0079 (11)
C7_10.0140 (13)0.0302 (15)0.0121 (11)0.0012 (10)0.0015 (10)0.0020 (10)
C8_10.0195 (13)0.0295 (14)0.0148 (12)0.0042 (11)0.0077 (10)0.0029 (11)
C9_10.0183 (13)0.0132 (13)0.0279 (14)0.0023 (10)0.0045 (11)0.0037 (11)
C10_10.0208 (13)0.0159 (13)0.0311 (14)0.0031 (11)0.0029 (11)0.0012 (11)
O1_10.0188 (9)0.0197 (9)0.0196 (8)0.0047 (7)0.0076 (7)0.0031 (7)
O2_10.0144 (8)0.0295 (10)0.0154 (8)0.0013 (7)0.0021 (7)0.0011 (7)
O3_10.0153 (9)0.0217 (9)0.0177 (8)0.0037 (7)0.0042 (7)0.0002 (7)
O4_10.0135 (8)0.0224 (9)0.0184 (9)0.0036 (7)0.0025 (7)0.0007 (7)
O5_10.0189 (9)0.0191 (9)0.0194 (8)0.0027 (7)0.0090 (7)0.0008 (7)
Ni1_10.00909 (14)0.01140 (15)0.00932 (13)0.00030 (12)0.00296 (10)0.00000 (12)
O6_10.0088 (8)0.0213 (9)0.0178 (8)0.0016 (8)0.0060 (6)0.0070 (8)
O7_10.0088 (7)0.0175 (10)0.0134 (7)0.0010 (7)0.0040 (6)0.0024 (7)
O8_10.0141 (8)0.0217 (9)0.0124 (8)0.0018 (7)0.0032 (7)0.0045 (7)
O9_10.0183 (8)0.0137 (8)0.0149 (8)0.0013 (7)0.0064 (7)0.0004 (7)
O10_10.0164 (8)0.0155 (8)0.0091 (7)0.0012 (7)0.0022 (6)0.0002 (6)
O11_10.0230 (9)0.0121 (8)0.0138 (8)0.0039 (7)0.0070 (7)0.0010 (7)
N1_10.0125 (10)0.0177 (11)0.0124 (9)0.0045 (8)0.0029 (8)0.0019 (8)
O12_10.0277 (10)0.0169 (9)0.0173 (8)0.0105 (8)0.0039 (7)0.0007 (7)
O13_10.0315 (10)0.0203 (9)0.0155 (8)0.0050 (8)0.0120 (7)0.0014 (7)
O14_10.0376 (11)0.0205 (10)0.0156 (9)0.0019 (8)0.0106 (8)0.0034 (8)
N2_10.0215 (11)0.0158 (11)0.0191 (11)0.0006 (9)0.0065 (9)0.0009 (9)
O15_10.0217 (9)0.0195 (9)0.0125 (8)0.0006 (7)0.0074 (7)0.0012 (7)
O16_10.0364 (11)0.0197 (9)0.0199 (9)0.0088 (8)0.0159 (8)0.0003 (7)
O17_10.0461 (12)0.0210 (10)0.0207 (10)0.0171 (9)0.0011 (9)0.0019 (8)
O18_10.048 (3)0.0225 (15)0.0205 (12)0.0138 (15)0.0145 (15)0.0064 (11)
O18'_10.048 (3)0.0225 (15)0.0205 (12)0.0138 (15)0.0145 (15)0.0064 (11)
C1_20.0221 (13)0.0279 (14)0.0144 (12)0.0022 (11)0.0056 (10)0.0051 (10)
C2_20.0105 (12)0.0260 (14)0.0141 (11)0.0015 (10)0.0011 (9)0.0009 (10)
C3_20.0243 (14)0.0219 (13)0.0201 (12)0.0012 (11)0.0020 (10)0.0079 (11)
C4_20.0178 (13)0.0196 (13)0.0262 (13)0.0052 (10)0.0004 (10)0.0046 (11)
C5_20.0154 (13)0.0169 (13)0.0310 (15)0.0010 (10)0.0106 (11)0.0072 (11)
C6_20.0167 (12)0.0241 (14)0.0227 (13)0.0055 (10)0.0060 (10)0.0086 (11)
C7_20.0151 (12)0.0326 (17)0.0121 (11)0.0037 (11)0.0037 (9)0.0017 (11)
C8_20.0189 (12)0.0267 (14)0.0160 (12)0.0011 (11)0.0082 (10)0.0033 (11)
C9_20.0168 (13)0.0106 (12)0.0245 (13)0.0019 (10)0.0039 (11)0.0016 (11)
C10_20.0194 (13)0.0134 (12)0.0246 (13)0.0029 (10)0.0072 (11)0.0026 (11)
O1_20.0206 (9)0.0192 (9)0.0165 (8)0.0032 (7)0.0084 (7)0.0015 (7)
O2_20.0156 (9)0.0230 (9)0.0177 (8)0.0002 (7)0.0020 (7)0.0016 (7)
O3_20.0161 (8)0.0189 (9)0.0194 (8)0.0025 (7)0.0034 (7)0.0004 (7)
O4_20.0134 (8)0.0189 (9)0.0203 (8)0.0018 (7)0.0021 (7)0.0024 (7)
O5_20.0160 (9)0.0181 (9)0.0187 (8)0.0006 (7)0.0076 (7)0.0010 (7)
Ni2_20.00941 (14)0.01073 (15)0.00942 (13)0.00003 (12)0.00296 (10)0.00057 (12)
O6_20.0090 (7)0.0162 (8)0.0198 (8)0.0015 (8)0.0063 (6)0.0057 (8)
O7_20.0094 (7)0.0152 (8)0.0124 (7)0.0001 (7)0.0031 (6)0.0025 (7)
O8_20.0118 (8)0.0203 (9)0.0126 (8)0.0000 (7)0.0029 (7)0.0060 (7)
O9_20.0201 (9)0.0122 (8)0.0130 (8)0.0007 (7)0.0057 (7)0.0008 (7)
O10_20.0155 (8)0.0129 (8)0.0127 (8)0.0009 (7)0.0029 (6)0.0006 (7)
O11_20.0207 (9)0.0132 (8)0.0127 (8)0.0032 (7)0.0058 (7)0.0010 (7)
N1_20.0148 (10)0.0196 (11)0.0130 (9)0.0025 (8)0.0018 (8)0.0004 (8)
O12_20.0196 (9)0.0175 (9)0.0171 (8)0.0003 (7)0.0046 (7)0.0006 (7)
O13_20.0397 (11)0.0195 (9)0.0140 (8)0.0002 (8)0.0120 (8)0.0007 (7)
O14_20.0576 (14)0.0234 (10)0.0186 (9)0.0153 (10)0.0172 (9)0.0021 (8)
N2_20.0200 (10)0.0121 (10)0.0177 (10)0.0013 (8)0.0065 (8)0.0020 (8)
O15_20.0236 (9)0.0184 (9)0.0149 (8)0.0016 (7)0.0094 (7)0.0016 (7)
O16_20.0299 (10)0.0158 (9)0.0181 (8)0.0076 (7)0.0110 (7)0.0004 (7)
O17_20.0373 (11)0.0210 (10)0.0202 (9)0.0143 (9)0.0043 (8)0.0020 (8)
O18_20.0592 (14)0.0280 (11)0.0218 (10)0.0090 (10)0.0141 (10)0.0084 (9)
Geometric parameters (Å, º) top
C1_1—O1_11.422 (3)O18'_1—H18D_10.98 (3)
C1_1—C2_11.509 (4)C1_2—O1_21.427 (3)
C1_1—H1A_10.9900C1_2—C2_21.503 (3)
C1_1—H1B_10.9900C1_2—H1A_20.9900
C2_1—O2_11.433 (3)C1_2—H1B_20.9900
C2_1—H2A_10.9900C2_2—O2_21.426 (3)
C2_1—H2B_10.9900C2_2—H2A_20.9900
C3_1—O2_11.435 (3)C2_2—H2B_20.9900
C3_1—C4_11.500 (3)C3_2—O2_21.434 (3)
C3_1—H3A_10.9900C3_2—C4_21.513 (3)
C3_1—H3B_10.9900C3_2—H3A_20.9900
C4_1—O3_11.426 (3)C3_2—H3B_20.9900
C4_1—H4A_10.9900C4_2—O3_21.422 (3)
C4_1—H4B_10.9900C4_2—H4A_20.9900
C5_1—O3_11.428 (3)C4_2—H4B_20.9900
C5_1—C6_11.500 (3)C5_2—O3_21.433 (3)
C5_1—H5A_10.9900C5_2—C6_21.493 (3)
C5_1—H5B_10.9900C5_2—H5A_20.9900
C6_1—O4_11.434 (3)C5_2—H5B_20.9900
C6_1—H6A_10.9900C6_2—O4_21.426 (3)
C6_1—H6B_10.9900C6_2—H6A_20.9900
C7_1—O4_11.427 (3)C6_2—H6B_20.9900
C7_1—C8_11.492 (3)C7_2—O4_21.435 (3)
C7_1—H7A_10.9900C7_2—C8_21.498 (3)
C7_1—H7B_10.9900C7_2—H7A_20.9900
C8_1—O5_11.430 (3)C7_2—H7B_20.9900
C8_1—H8A_10.9900C8_2—O5_21.431 (3)
C8_1—H8B_10.9900C8_2—H8A_20.9900
C9_1—O5_11.424 (3)C8_2—H8B_20.9900
C9_1—C10_11.496 (3)C9_2—O5_21.433 (3)
C9_1—H9A_10.9900C9_2—C10_21.504 (3)
C9_1—H9B_10.9900C9_2—H9A_20.9900
C10_1—O1_11.433 (3)C9_2—H9B_20.9900
C10_1—H10A_10.9900C10_2—O1_21.428 (3)
C10_1—H10B_10.9900C10_2—H10A_20.9900
Ni1_1—O7_12.0416 (15)C10_2—H10B_20.9900
Ni1_1—O6_12.0436 (14)Ni2_2—O7_22.0355 (14)
Ni1_1—O8_12.0440 (15)Ni2_2—O11_22.0459 (16)
Ni1_1—O11_12.0529 (16)Ni2_2—O6_22.0479 (14)
Ni1_1—O10_12.0613 (15)Ni2_2—O8_22.0515 (15)
Ni1_1—O9_12.0707 (16)Ni2_2—O9_22.0538 (16)
O6_1—H6C_10.831 (9)Ni2_2—O10_22.0660 (15)
O6_1—H6D_10.838 (9)O6_2—H6C_20.832 (9)
O7_1—H7C_10.833 (9)O6_2—H6D_20.827 (9)
O7_1—H7D_10.839 (9)O7_2—H7C_20.843 (9)
O8_1—H8C_10.828 (9)O7_2—H7D_20.847 (9)
O8_1—H8D_10.840 (9)O8_2—H8C_20.832 (9)
O9_1—H9C_10.830 (9)O8_2—H8D_20.836 (9)
O9_1—H9D_10.842 (9)O9_2—H9C_20.832 (9)
O10_1—H10C_10.848 (9)O9_2—H9D_20.830 (9)
O10_1—H10D_10.852 (9)O10_2—H10C_20.848 (9)
O11_1—H11C_10.829 (9)O10_2—H10D_20.842 (9)
O11_1—H11D_10.835 (9)O11_2—H11C_20.842 (9)
N1_1—O14_11.243 (2)O11_2—H11D_20.841 (9)
N1_1—O12_11.250 (2)N1_2—O14_21.240 (2)
N1_1—O13_11.256 (2)N1_2—O13_21.248 (2)
N2_1—O16_11.251 (2)N1_2—O12_21.256 (3)
N2_1—O15_11.251 (2)N2_2—O15_21.247 (2)
N2_1—O17_11.255 (3)N2_2—O16_21.253 (2)
O18_1—H18C_10.840 (10)N2_2—O17_21.257 (3)
O18_1—H18D_10.838 (10)O18_2—H18C_20.858 (10)
O18'_1—H18C_10.84 (3)O18_2—H18D_20.845 (10)
O1_1—C1_1—C2_1108.12 (19)O1_2—C1_2—C2_2108.21 (19)
O1_1—C1_1—H1A_1110.1O1_2—C1_2—H1A_2110.1
C2_1—C1_1—H1A_1110.1C2_2—C1_2—H1A_2110.1
O1_1—C1_1—H1B_1110.1O1_2—C1_2—H1B_2110.1
C2_1—C1_1—H1B_1110.1C2_2—C1_2—H1B_2110.1
H1A_1—C1_1—H1B_1108.4H1A_2—C1_2—H1B_2108.4
O2_1—C2_1—C1_1109.68 (19)O2_2—C2_2—C1_2109.17 (19)
O2_1—C2_1—H2A_1109.7O2_2—C2_2—H2A_2109.8
C1_1—C2_1—H2A_1109.7C1_2—C2_2—H2A_2109.8
O2_1—C2_1—H2B_1109.7O2_2—C2_2—H2B_2109.8
C1_1—C2_1—H2B_1109.7C1_2—C2_2—H2B_2109.8
H2A_1—C2_1—H2B_1108.2H2A_2—C2_2—H2B_2108.3
O2_1—C3_1—C4_1112.28 (19)O2_2—C3_2—C4_2111.85 (19)
O2_1—C3_1—H3A_1109.1O2_2—C3_2—H3A_2109.2
C4_1—C3_1—H3A_1109.1C4_2—C3_2—H3A_2109.2
O2_1—C3_1—H3B_1109.1O2_2—C3_2—H3B_2109.2
C4_1—C3_1—H3B_1109.1C4_2—C3_2—H3B_2109.2
H3A_1—C3_1—H3B_1107.9H3A_2—C3_2—H3B_2107.9
O3_1—C4_1—C3_1108.13 (19)O3_2—C4_2—C3_2107.79 (19)
O3_1—C4_1—H4A_1110.1O3_2—C4_2—H4A_2110.1
C3_1—C4_1—H4A_1110.1C3_2—C4_2—H4A_2110.1
O3_1—C4_1—H4B_1110.1O3_2—C4_2—H4B_2110.1
C3_1—C4_1—H4B_1110.1C3_2—C4_2—H4B_2110.1
H4A_1—C4_1—H4B_1108.4H4A_2—C4_2—H4B_2108.5
O3_1—C5_1—C6_1108.8 (2)O3_2—C5_2—C6_2108.8 (2)
O3_1—C5_1—H5A_1109.9O3_2—C5_2—H5A_2109.9
C6_1—C5_1—H5A_1109.9C6_2—C5_2—H5A_2109.9
O3_1—C5_1—H5B_1109.9O3_2—C5_2—H5B_2109.9
C6_1—C5_1—H5B_1109.9C6_2—C5_2—H5B_2109.9
H5A_1—C5_1—H5B_1108.3H5A_2—C5_2—H5B_2108.3
O4_1—C6_1—C5_1108.09 (19)O4_2—C6_2—C5_2108.26 (19)
O4_1—C6_1—H6A_1110.1O4_2—C6_2—H6A_2110.0
C5_1—C6_1—H6A_1110.1C5_2—C6_2—H6A_2110.0
O4_1—C6_1—H6B_1110.1O4_2—C6_2—H6B_2110.0
C5_1—C6_1—H6B_1110.1C5_2—C6_2—H6B_2110.0
H6A_1—C6_1—H6B_1108.4H6A_2—C6_2—H6B_2108.4
O4_1—C7_1—C8_1108.04 (19)O4_2—C7_2—C8_2108.00 (18)
O4_1—C7_1—H7A_1110.1O4_2—C7_2—H7A_2110.1
C8_1—C7_1—H7A_1110.1C8_2—C7_2—H7A_2110.1
O4_1—C7_1—H7B_1110.1O4_2—C7_2—H7B_2110.1
C8_1—C7_1—H7B_1110.1C8_2—C7_2—H7B_2110.1
H7A_1—C7_1—H7B_1108.4H7A_2—C7_2—H7B_2108.4
O5_1—C8_1—C7_1108.58 (19)O5_2—C8_2—C7_2106.59 (18)
O5_1—C8_1—H8A_1110.0O5_2—C8_2—H8A_2110.4
C7_1—C8_1—H8A_1110.0C7_2—C8_2—H8A_2110.4
O5_1—C8_1—H8B_1110.0O5_2—C8_2—H8B_2110.4
C7_1—C8_1—H8B_1110.0C7_2—C8_2—H8B_2110.4
H8A_1—C8_1—H8B_1108.4H8A_2—C8_2—H8B_2108.6
O5_1—C9_1—C10_1107.74 (19)O5_2—C9_2—C10_2107.94 (19)
O5_1—C9_1—H9A_1110.2O5_2—C9_2—H9A_2110.1
C10_1—C9_1—H9A_1110.2C10_2—C9_2—H9A_2110.1
O5_1—C9_1—H9B_1110.2O5_2—C9_2—H9B_2110.1
C10_1—C9_1—H9B_1110.2C10_2—C9_2—H9B_2110.1
H9A_1—C9_1—H9B_1108.5H9A_2—C9_2—H9B_2108.4
O1_1—C10_1—C9_1108.2 (2)O1_2—C10_2—C9_2107.52 (19)
O1_1—C10_1—H10A_1110.1O1_2—C10_2—H10A_2110.2
C9_1—C10_1—H10A_1110.1C9_2—C10_2—H10A_2110.2
O1_1—C10_1—H10B_1110.1O1_2—C10_2—H10B_2110.2
C9_1—C10_1—H10B_1110.1C9_2—C10_2—H10B_2110.2
H10A_1—C10_1—H10B_1108.4H10A_2—C10_2—H10B_2108.5
C1_1—O1_1—C10_1113.51 (19)C1_2—O1_2—C10_2112.88 (17)
C2_1—O2_1—C3_1114.08 (18)C2_2—O2_2—C3_2112.93 (18)
C4_1—O3_1—C5_1112.01 (18)C4_2—O3_2—C5_2112.77 (18)
C7_1—O4_1—C6_1114.36 (18)C6_2—O4_2—C7_2115.25 (17)
C9_1—O5_1—C8_1114.37 (18)C8_2—O5_2—C9_2114.63 (17)
O7_1—Ni1_1—O6_1173.47 (8)O7_2—Ni2_2—O11_290.16 (7)
O7_1—Ni1_1—O8_188.48 (6)O7_2—Ni2_2—O6_2174.76 (8)
O6_1—Ni1_1—O8_187.50 (6)O11_2—Ni2_2—O6_293.57 (7)
O7_1—Ni1_1—O11_190.35 (7)O7_2—Ni2_2—O8_289.39 (6)
O6_1—Ni1_1—O11_194.72 (7)O11_2—Ni2_2—O8_290.60 (6)
O8_1—Ni1_1—O11_188.92 (7)O6_2—Ni2_2—O8_286.90 (6)
O7_1—Ni1_1—O10_193.11 (6)O7_2—Ni2_2—O9_285.78 (7)
O6_1—Ni1_1—O10_191.22 (6)O11_2—Ni2_2—O9_2173.39 (6)
O8_1—Ni1_1—O10_1176.17 (7)O6_2—Ni2_2—O9_290.83 (7)
O11_1—Ni1_1—O10_187.59 (6)O8_2—Ni2_2—O9_294.56 (6)
O7_1—Ni1_1—O9_185.65 (6)O7_2—Ni2_2—O10_292.51 (6)
O6_1—Ni1_1—O9_189.54 (7)O11_2—Ni2_2—O10_287.93 (6)
O8_1—Ni1_1—O9_194.66 (6)O6_2—Ni2_2—O10_291.30 (6)
O11_1—Ni1_1—O9_1174.55 (7)O8_2—Ni2_2—O10_2177.61 (6)
O10_1—Ni1_1—O9_188.94 (6)O9_2—Ni2_2—O10_287.04 (6)
Ni1_1—O6_1—H6C_1123.2 (16)Ni2_2—O6_2—H6C_2121.4 (16)
Ni1_1—O6_1—H6D_1131.2 (15)Ni2_2—O6_2—H6D_2132.6 (16)
H6C_1—O6_1—H6D_1105.0 (14)H6C_2—O6_2—H6D_2105.6 (14)
Ni1_1—O7_1—H7C_1115.5 (15)Ni2_2—O7_2—H7C_2115.9 (15)
Ni1_1—O7_1—H7D_1124.2 (16)Ni2_2—O7_2—H7D_2123.9 (16)
H7C_1—O7_1—H7D_1104.3 (14)H7C_2—O7_2—H7D_2101.6 (13)
Ni1_1—O8_1—H8C_1117.1 (16)Ni2_2—O8_2—H8C_2115.2 (16)
Ni1_1—O8_1—H8D_1130.0 (16)Ni2_2—O8_2—H8D_2122.8 (16)
H8C_1—O8_1—H8D_1105.3 (14)H8C_2—O8_2—H8D_2104.8 (14)
Ni1_1—O9_1—H9C_1110.8 (18)Ni2_2—O9_2—H9C_2113.5 (17)
Ni1_1—O9_1—H9D_1119.4 (18)Ni2_2—O9_2—H9D_2123.4 (17)
H9C_1—O9_1—H9D_1104.4 (14)H9C_2—O9_2—H9D_2106.2 (14)
Ni1_1—O10_1—H10C_1116.2 (16)Ni2_2—O10_2—H10C_2111.2 (16)
Ni1_1—O10_1—H10D_1123.1 (16)Ni2_2—O10_2—H10D_2116.8 (17)
H10C_1—O10_1—H10D_1101.5 (13)H10C_2—O10_2—H10D_2102.6 (13)
Ni1_1—O11_1—H11C_1109.0 (17)Ni2_2—O11_2—H11C_2112.8 (17)
Ni1_1—O11_1—H11D_1123.9 (18)Ni2_2—O11_2—H11D_2122.6 (17)
H11C_1—O11_1—H11D_1105.8 (14)H11C_2—O11_2—H11D_2103.5 (14)
O14_1—N1_1—O12_1120.75 (19)O14_2—N1_2—O13_2121.0 (2)
O14_1—N1_1—O13_1120.27 (19)O14_2—N1_2—O12_2119.83 (19)
O12_1—N1_1—O13_1118.98 (18)O13_2—N1_2—O12_2119.21 (19)
O16_1—N2_1—O15_1120.01 (19)O15_2—N2_2—O16_2119.90 (18)
O16_1—N2_1—O17_1119.40 (19)O15_2—N2_2—O17_2121.22 (19)
O15_1—N2_1—O17_1120.59 (19)O16_2—N2_2—O17_2118.88 (18)
H18C_1—O18_1—H18D_1103.6 (15)H18C_2—O18_2—H18D_2101.3 (14)
H18C_1—O18'_1—H18D_193 (3)
O1_1—C1_1—C2_1—O2_176.8 (2)O1_2—C1_2—C2_2—O2_278.1 (2)
O2_1—C3_1—C4_1—O3_158.0 (3)O2_2—C3_2—C4_2—O3_255.9 (3)
O3_1—C5_1—C6_1—O4_171.5 (2)O3_2—C5_2—C6_2—O4_273.7 (2)
O4_1—C7_1—C8_1—O5_166.3 (2)O4_2—C7_2—C8_2—O5_268.9 (2)
O5_1—C9_1—C10_1—O1_161.5 (3)O5_2—C9_2—C10_2—O1_261.4 (2)
C2_1—C1_1—O1_1—C10_1171.00 (19)C2_2—C1_2—O1_2—C10_2166.98 (19)
C9_1—C10_1—O1_1—C1_1175.4 (2)C9_2—C10_2—O1_2—C1_2179.02 (19)
C1_1—C2_1—O2_1—C3_1166.25 (18)C1_2—C2_2—O2_2—C3_2167.92 (19)
C4_1—C3_1—O2_1—C2_181.7 (2)C4_2—C3_2—O2_2—C2_280.9 (2)
C3_1—C4_1—O3_1—C5_1174.5 (2)C3_2—C4_2—O3_2—C5_2171.76 (19)
C6_1—C5_1—O3_1—C4_1164.26 (19)C6_2—C5_2—O3_2—C4_2164.72 (19)
C8_1—C7_1—O4_1—C6_1170.02 (18)C5_2—C6_2—O4_2—C7_2163.88 (18)
C5_1—C6_1—O4_1—C7_1161.47 (19)C8_2—C7_2—O4_2—C6_2164.98 (19)
C10_1—C9_1—O5_1—C8_1167.88 (19)C7_2—C8_2—O5_2—C9_2164.03 (19)
C7_1—C8_1—O5_1—C9_1156.52 (19)C10_2—C9_2—O5_2—C8_2165.29 (19)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6_1—H6C_1···O3_10.83 (1)2.05 (1)2.876 (2)173 (3)
O6_1—H6D_1···O5_10.84 (1)1.90 (1)2.730 (2)170 (3)
O7_1—H7C_1···O4_20.83 (1)1.93 (1)2.757 (2)176 (3)
O7_1—H7D_1···O1_20.84 (1)1.93 (1)2.762 (2)171 (2)
O8_1—H8C_1···O2_10.83 (1)2.02 (1)2.841 (2)169 (2)
O8_1—H8D_1···O13_2i0.84 (1)2.00 (1)2.832 (2)174 (3)
O9_1—H9C_1···O16_1ii0.83 (1)1.94 (1)2.763 (2)174 (3)
O9_1—H9D_1···O14_10.84 (1)2.03 (1)2.860 (2)169 (2)
O10_1—H10C_1···O12_10.85 (1)1.91 (1)2.742 (2)167 (2)
O10_1—H10D_1···O17_10.85 (1)1.92 (1)2.766 (2)174 (2)
O11_1—H11C_1···O15_10.83 (1)1.99 (1)2.782 (2)161 (3)
O11_1—H11D_1···O18_10.84 (1)1.87 (1)2.703 (3)177 (2)
O6_2—H6C_2···O3_20.83 (1)2.01 (1)2.828 (2)167 (3)
O6_2—H6D_2···O5_20.83 (1)1.92 (1)2.746 (2)179 (3)
O7_2—H7C_2···O4_1iii0.84 (1)1.94 (1)2.772 (2)171 (2)
O7_2—H7D_2···O1_1iii0.85 (1)1.90 (1)2.740 (2)170 (2)
O8_2—H8C_2···O2_20.83 (1)1.99 (1)2.821 (2)177 (3)
O8_2—H8D_2···O13_1iv0.84 (1)2.03 (1)2.840 (2)163 (2)
O9_2—H9C_2···O16_2v0.83 (1)1.89 (1)2.712 (2)172 (3)
O9_2—H9D_2···O14_20.83 (1)2.00 (1)2.819 (2)170 (2)
O10_2—H10C_2···O12_20.85 (1)1.92 (1)2.742 (2)165 (2)
O10_2—H10D_2···O17_20.84 (1)1.90 (1)2.722 (2)167 (2)
O11_2—H11C_2···O15_20.84 (1)1.93 (1)2.764 (2)170 (3)
O11_2—H11D_2···O18_20.84 (1)1.86 (1)2.697 (2)177 (3)
O18_2—H18D_2···O13_2vi0.85 (1)2.09 (1)2.930 (3)179 (4)
Symmetry codes: (i) x1/2, y, z1/2; (ii) x+1/2, y+1/2, z+1/2; (iii) x+1, y, z; (iv) x+1/2, y, z1/2; (v) x+3/2, y+1/2, z+1/2; (vi) x+3/2, y1/2, z+1/2.
(2b) top
Crystal data top
C10H20O5·H12NiO62+·2(NO3)·H2OZ = 6
Mr = 529.10F(000) = 1680
Triclinic, P1Dx = 1.564 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 16.036 (1) ÅCell parameters from 11233 reflections
b = 24.765 (2) Åθ = 1.0–27.5°
c = 10.163 (1) ŵ = 0.95 mm1
α = 89.71 (1)°T = 90 K
β = 122.53 (1)°Irregular block, pale green
γ = 83.58 (1)°0.20 × 0.15 × 0.10 mm
V = 3371.2 (6) Å3
Data collection top
Nonius KappaCCD
diffractometer
15437 independent reflections
Radiation source: fine-focus sealed tube8504 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.000
Detector resolution: 18 pixels mm-1θmax = 27.5°, θmin = 1.5°
ω scans at fixed χ = 55°h = 2020
Absorption correction: multi-scan
Scalepack (Otwinowski & Minor, 2006)
k = 032
Tmin = 0.833, Tmax = 0.911l = 1313
15437 measured reflections
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)] = 0.064Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.159H atoms treated by a mixture of independent and constrained refinement
S = 1.02 w = 1/[σ2(Fo2) + (0.0579P)2 + 6.1685P]
where P = (Fo2 + 2Fc2)/3
15437 reflections(Δ/σ)max = 0.001
980 parametersΔρmax = 2.08 e Å3
71 restraintsΔρmin = 0.74 e Å3
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C1_10.2790 (4)0.2665 (2)0.2989 (6)0.0313 (12)
H1A_10.21870.25670.29230.038*
H1B_10.29730.24010.24280.038*
C2_10.2581 (4)0.3233 (2)0.2257 (6)0.0302 (12)
H2A_10.32110.33590.25040.036*
H2B_10.21310.32390.11050.036*
C3_10.2076 (4)0.4152 (2)0.2534 (6)0.0311 (12)
H3A_10.15410.43590.26130.037*
H3B_10.18960.42110.14430.037*
C4_10.3031 (4)0.4368 (2)0.3603 (6)0.0307 (13)
H4A_10.35640.41820.34840.037*
H4B_10.29540.47630.33350.037*
C5_10.4170 (4)0.45132 (19)0.6273 (6)0.0278 (12)
H5A_10.40000.49130.62170.033*
H5B_10.46820.44400.60100.033*
C6_10.4572 (4)0.42710 (18)0.7893 (6)0.0279 (12)
H6A_10.50800.44840.86790.033*
H6B_10.40270.42760.80820.033*
C7_10.5212 (4)0.33931 (19)0.9340 (6)0.0272 (12)
H7A_10.46340.34490.94540.033*
H7B_10.58030.34941.03060.033*
C8_10.5404 (4)0.28075 (19)0.9077 (6)0.0282 (12)
H8A_10.59380.27610.88580.034*
H8B_10.56230.25711.00260.034*
C9_10.4647 (4)0.21859 (19)0.7091 (6)0.0281 (12)
H9A_10.47740.18540.77530.034*
H9B_10.52290.21980.70020.034*
C10_10.3723 (4)0.21719 (18)0.5500 (6)0.0261 (12)
H10A_10.37960.18420.50060.031*
H10B_10.31380.21640.55840.031*
O1_10.3591 (2)0.26482 (12)0.4585 (4)0.0266 (8)
O2_10.2120 (2)0.35837 (13)0.2873 (4)0.0295 (8)
O3_10.3299 (2)0.42777 (12)0.5185 (4)0.0245 (8)
O4_10.5012 (2)0.37206 (12)0.8018 (4)0.0252 (8)
O5_10.4504 (2)0.26596 (12)0.7782 (4)0.0227 (7)
Ni1_10.15027 (4)0.34278 (2)0.62164 (7)0.02277 (16)
O6_10.2848 (2)0.34488 (13)0.6480 (4)0.0263 (8)
H6C_10.291 (3)0.3683 (14)0.595 (5)0.039*
H6D_10.329 (3)0.3193 (13)0.671 (6)0.039*
O7_10.0096 (2)0.34550 (13)0.5774 (4)0.0249 (8)
H7C_10.022 (3)0.3197 (15)0.537 (5)0.037*
H7D_10.012 (3)0.3590 (17)0.630 (5)0.037*
O8_10.0817 (3)0.34957 (18)0.3832 (4)0.0432 (10)
H8C_10.119 (3)0.348 (2)0.348 (6)0.065*
H8D_10.033 (3)0.372 (2)0.321 (6)0.065*
O9_10.1420 (4)0.42601 (16)0.6349 (6)0.0561 (13)
H9C_10.089 (3)0.447 (2)0.582 (6)0.084*
H9D_10.160 (5)0.431 (3)0.729 (3)0.084*
O10_10.2212 (2)0.33229 (15)0.8613 (4)0.0303 (8)
H10C_10.254 (3)0.3576 (12)0.908 (6)0.045*
H10D_10.261 (3)0.3035 (11)0.906 (6)0.045*
O11_10.1580 (2)0.26040 (13)0.6186 (4)0.0261 (8)
H11C_10.134 (3)0.2432 (17)0.538 (3)0.039*
H11D_10.206 (3)0.2382 (16)0.688 (4)0.039*
N1_10.3843 (3)0.43690 (18)1.0881 (5)0.0305 (10)
O12_10.3816 (3)0.38606 (14)1.0931 (4)0.0342 (9)
O13_10.4425 (3)0.45868 (14)1.2100 (4)0.0344 (9)
O14_10.3269 (3)0.46528 (16)0.9633 (4)0.0472 (11)
N2_10.3915 (3)0.20732 (17)0.9679 (5)0.0293 (10)
O15_10.3209 (3)0.19180 (13)0.8469 (4)0.0286 (8)
O16_10.4752 (3)0.17882 (13)1.0371 (4)0.0329 (9)
O17_10.3794 (3)0.25089 (14)1.0224 (4)0.0356 (9)
N3_10.0710 (8)0.4708 (4)0.1906 (13)0.0286 (14)0.529 (6)
O19_10.0550 (7)0.4235 (3)0.1597 (11)0.0384 (17)0.529 (6)
O20_10.0306 (18)0.4818 (8)0.3291 (12)0.035 (3)0.529 (6)
O21_10.1278 (7)0.5067 (4)0.0813 (10)0.0471 (19)0.529 (6)
N3'_10.0693 (9)0.4817 (4)0.1946 (14)0.0286 (14)0.471 (6)
O19'_10.0807 (8)0.4482 (4)0.0964 (12)0.0384 (17)0.471 (6)
O20'_10.011 (2)0.4677 (9)0.3363 (13)0.035 (3)0.471 (6)
O21'_10.1168 (8)0.5289 (4)0.1504 (12)0.0471 (19)0.471 (6)
O18_10.1026 (3)0.20811 (16)0.3581 (5)0.0451 (10)
H18C_10.080 (4)0.194 (2)0.406 (5)0.068*
H18D_10.056 (3)0.207 (3)0.2636 (19)0.068*
C1_20.8302 (4)0.2537 (2)0.3078 (6)0.0300 (12)
H1A_20.76830.24450.29680.036*
H1B_20.85300.22540.26130.036*
C2_20.8106 (4)0.3084 (2)0.2261 (6)0.0307 (12)
H2A_20.87400.31960.24800.037*
H2B_20.76560.30680.11160.037*
C3_20.7742 (4)0.4017 (2)0.2496 (6)0.0349 (13)
H3A_20.74520.40920.13630.042*
H3B_20.84540.40700.30720.042*
C4_20.7195 (4)0.4393 (2)0.3013 (6)0.0323 (13)
H4A_20.72470.47740.28010.039*
H4B_20.64790.43460.23970.039*
C5_20.8431 (4)0.45550 (19)0.5653 (6)0.0280 (12)
H5A_20.82360.49540.55340.034*
H5B_20.89360.44780.53770.034*
C6_20.8864 (4)0.43424 (19)0.7320 (6)0.0288 (12)
H6A_20.93330.45830.80550.035*
H6B_20.83240.43320.75170.035*
C7_20.9661 (4)0.35126 (19)0.8967 (6)0.0288 (12)
H7A_20.90670.34840.90140.035*
H7B_21.01310.37040.98760.035*
C8_21.0152 (3)0.2957 (2)0.9001 (6)0.0268 (12)
H8A_21.07440.29880.89490.032*
H8B_21.03740.27430.99870.032*
C9_20.9881 (4)0.22267 (19)0.7336 (6)0.0274 (12)
H9A_21.00170.19070.80450.033*
H9B_21.05200.22960.74780.033*
C10_20.9169 (4)0.21163 (19)0.5684 (6)0.0271 (12)
H10A_20.94260.17760.54380.033*
H10B_20.85160.20710.55260.033*
O1_20.9051 (2)0.25586 (13)0.4684 (4)0.0259 (8)
O2_20.7652 (2)0.34684 (13)0.2813 (4)0.0279 (8)
O3_20.7580 (2)0.42952 (13)0.4644 (4)0.0271 (8)
O4_20.9376 (2)0.38054 (13)0.7545 (4)0.0290 (8)
O5_20.9450 (2)0.26934 (12)0.7696 (4)0.0226 (7)
Ni2_20.62237 (4)0.32005 (2)0.54131 (7)0.01885 (15)
O6_20.7467 (2)0.30770 (14)0.5296 (4)0.0244 (8)
H6C_20.8080 (17)0.304 (2)0.603 (3)0.037*
H6D_20.749 (3)0.319 (2)0.453 (3)0.037*
O7_20.4962 (2)0.33451 (13)0.5435 (4)0.0213 (7)
H7C_20.505 (3)0.3432 (19)0.629 (3)0.032*
H7D_20.451 (3)0.3149 (17)0.510 (5)0.032*
O8_20.5373 (2)0.30468 (14)0.3082 (4)0.0292 (8)
H8C_20.498 (3)0.3301 (12)0.248 (5)0.044*
H8D_20.519 (4)0.2759 (10)0.270 (5)0.044*
O9_20.6033 (2)0.40150 (13)0.4837 (4)0.0253 (8)
H9C_20.556 (2)0.4151 (19)0.394 (3)0.038*
H9D_20.653 (2)0.4122 (19)0.492 (5)0.038*
O10_20.7059 (2)0.33529 (13)0.7716 (4)0.0279 (8)
H10C_20.749 (3)0.3127 (14)0.841 (4)0.042*
H10D_20.706 (4)0.3643 (11)0.814 (5)0.042*
O11_20.6428 (2)0.24089 (12)0.6165 (4)0.0238 (7)
H11C_20.699 (2)0.2215 (17)0.674 (4)0.036*
H11D_20.612 (3)0.2243 (17)0.536 (3)0.036*
N1_20.8786 (3)0.20335 (16)0.9464 (5)0.0238 (9)
O12_20.8294 (2)0.18434 (12)0.8163 (4)0.0253 (8)
O13_20.9631 (3)0.17879 (13)1.0491 (4)0.0342 (9)
O14_20.8467 (3)0.24665 (13)0.9771 (4)0.0341 (9)
N2_20.5444 (3)0.14610 (16)0.3622 (5)0.0279 (10)
O15_20.5035 (3)0.18818 (14)0.3853 (4)0.0401 (10)
O16_20.4926 (2)0.10942 (13)0.2896 (4)0.0259 (8)
O17_20.6350 (2)0.14147 (15)0.4125 (4)0.0373 (9)
O18_20.7175 (3)0.43898 (14)0.8631 (4)0.0364 (9)
H18C_20.7697 (19)0.449 (2)0.937 (5)0.055*
H18D_20.672 (2)0.4630 (16)0.849 (6)0.055*
C1_30.3655 (3)0.02904 (19)0.3486 (6)0.0249 (11)
H1A_30.39050.04380.45190.030*
H1B_30.40890.03760.31190.030*
C2_30.3677 (4)0.03137 (19)0.3629 (6)0.0267 (11)
H2A_30.43080.04780.45830.032*
H2B_30.31140.03980.37040.032*
C3_30.3374 (4)0.10797 (18)0.2083 (6)0.0280 (12)
H3A_30.27860.11070.21480.034*
H3B_30.39470.13280.29290.034*
C4_30.3164 (4)0.1238 (2)0.0541 (6)0.0286 (12)
H4A_30.37290.11800.04390.034*
H4B_30.30800.16290.04420.034*
C5_30.2147 (4)0.0882 (2)0.2158 (6)0.0305 (12)
H5A_30.19120.12180.26850.037*
H5B_30.27910.08430.20410.037*
C6_30.1388 (4)0.03938 (19)0.3110 (6)0.0281 (12)
H6A_30.12600.03690.41780.034*
H6B_30.07510.04250.31960.034*
C7_30.1114 (3)0.05682 (19)0.3062 (6)0.0244 (11)
H7A_30.04970.05480.30750.029*
H7B_30.09320.06240.41560.029*
C8_30.1625 (4)0.10310 (19)0.2146 (6)0.0246 (11)
H8A_30.23080.10020.19350.030*
H8B_30.12500.13830.27540.030*
C9_30.2522 (4)0.1225 (2)0.0562 (6)0.0267 (12)
H9A_30.24590.16240.03530.032*
H9B_30.31450.10520.06720.032*
C10_30.2545 (4)0.11071 (18)0.2022 (6)0.0256 (11)
H10A_30.31100.12630.29030.031*
H10B_30.19210.12870.18980.031*
O1_30.2650 (2)0.05326 (12)0.2394 (4)0.0261 (8)
O2_30.3597 (2)0.05312 (12)0.2262 (4)0.0246 (8)
O3_30.2268 (2)0.09107 (13)0.0662 (4)0.0275 (8)
O4_30.1788 (2)0.00773 (13)0.2328 (4)0.0268 (8)
O5_30.1670 (2)0.10086 (13)0.0709 (4)0.0239 (8)
Ni3_30.00000.00000.00000.0171 (2)
O6_30.1414 (2)0.01993 (13)0.0544 (4)0.0223 (7)
H6C_30.180 (3)0.0034 (15)0.099 (5)0.033*
H6D_30.162 (3)0.0369 (16)0.007 (5)0.033*
O8_30.0094 (2)0.08018 (12)0.0401 (4)0.0229 (7)
H8C_30.059 (2)0.0863 (17)0.042 (6)0.034*
H8D_30.008 (3)0.1090 (13)0.014 (6)0.034*
O9_30.0544 (2)0.00654 (13)0.2317 (4)0.0214 (7)
H9C_30.082 (3)0.0344 (10)0.272 (5)0.032*
H9D_30.097 (3)0.0195 (11)0.289 (5)0.032*
Ni4_30.50000.00000.00000.0182 (2)
O7_30.6242 (2)0.00758 (13)0.0129 (4)0.0236 (8)
H7C_30.680 (2)0.005 (2)0.069 (3)0.035*
H7D_30.622 (3)0.0122 (17)0.082 (4)0.035*
O10_30.4206 (3)0.02794 (15)0.2143 (4)0.0361 (9)
H10C_30.373 (3)0.0094 (18)0.294 (4)0.054*
H10D_30.436 (4)0.0549 (14)0.251 (5)0.054*
O11_30.4580 (2)0.07835 (12)0.1048 (4)0.0246 (8)
H11C_30.413 (3)0.0858 (18)0.199 (2)0.037*
H11D_30.461 (3)0.1075 (13)0.062 (4)0.037*
N1_30.2312 (3)0.07350 (16)0.5055 (5)0.0240 (9)
O12_30.2489 (2)0.02283 (13)0.5351 (4)0.0283 (8)
O13_30.2959 (3)0.10350 (14)0.5829 (4)0.0330 (9)
O14_30.1451 (2)0.09433 (13)0.3932 (4)0.0262 (8)
O18_30.1601 (3)0.09401 (13)0.3819 (4)0.0285 (8)
H18C_30.2216 (10)0.1029 (19)0.439 (4)0.043*
H18D_30.141 (3)0.1126 (18)0.306 (4)0.043*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C1_10.033 (3)0.035 (3)0.028 (3)0.012 (2)0.016 (3)0.009 (2)
C2_10.033 (3)0.039 (3)0.027 (3)0.010 (2)0.021 (3)0.008 (2)
C3_10.028 (3)0.032 (3)0.034 (3)0.004 (2)0.019 (3)0.008 (2)
C4_10.038 (3)0.022 (3)0.038 (3)0.002 (2)0.026 (3)0.010 (2)
C5_10.032 (3)0.016 (2)0.041 (3)0.004 (2)0.023 (3)0.001 (2)
C6_10.039 (3)0.016 (3)0.036 (3)0.003 (2)0.025 (3)0.009 (2)
C7_10.023 (3)0.031 (3)0.020 (3)0.004 (2)0.007 (2)0.001 (2)
C8_10.022 (3)0.024 (3)0.033 (3)0.000 (2)0.012 (3)0.004 (2)
C9_10.029 (3)0.022 (3)0.036 (3)0.006 (2)0.021 (3)0.003 (2)
C10_10.034 (3)0.018 (3)0.035 (3)0.007 (2)0.024 (3)0.007 (2)
O1_10.0267 (19)0.0218 (18)0.030 (2)0.0069 (15)0.0140 (18)0.0028 (15)
O2_10.028 (2)0.030 (2)0.034 (2)0.0013 (16)0.0191 (18)0.0026 (16)
O3_10.0258 (19)0.0208 (18)0.029 (2)0.0014 (14)0.0167 (17)0.0041 (15)
O4_10.0294 (19)0.0206 (18)0.032 (2)0.0023 (15)0.0213 (18)0.0017 (15)
O5_10.0199 (18)0.0168 (17)0.030 (2)0.0034 (14)0.0135 (17)0.0003 (15)
Ni1_10.0204 (3)0.0214 (3)0.0297 (4)0.0008 (3)0.0163 (3)0.0018 (3)
O6_10.0230 (19)0.0214 (19)0.039 (2)0.0021 (14)0.0209 (18)0.0063 (16)
O7_10.0204 (19)0.0253 (19)0.035 (2)0.0008 (15)0.0198 (18)0.0018 (16)
O8_10.022 (2)0.074 (3)0.029 (2)0.0028 (19)0.0108 (19)0.017 (2)
O9_10.062 (3)0.021 (2)0.116 (4)0.003 (2)0.070 (3)0.006 (3)
O10_10.028 (2)0.036 (2)0.030 (2)0.0073 (16)0.0173 (18)0.0110 (18)
O11_10.024 (2)0.0230 (19)0.027 (2)0.0014 (15)0.0115 (17)0.0035 (15)
N1_10.036 (3)0.035 (3)0.030 (3)0.002 (2)0.025 (2)0.000 (2)
O12_10.039 (2)0.024 (2)0.038 (2)0.0001 (17)0.020 (2)0.0035 (17)
O13_10.034 (2)0.028 (2)0.037 (2)0.0105 (17)0.016 (2)0.0035 (18)
O14_10.051 (3)0.049 (3)0.030 (2)0.017 (2)0.019 (2)0.017 (2)
N2_10.032 (3)0.024 (2)0.036 (3)0.001 (2)0.021 (2)0.007 (2)
O15_10.028 (2)0.0230 (19)0.030 (2)0.0054 (16)0.0120 (18)0.0012 (16)
O16_10.029 (2)0.029 (2)0.037 (2)0.0072 (16)0.0176 (19)0.0098 (17)
O17_10.038 (2)0.028 (2)0.034 (2)0.0025 (17)0.0170 (19)0.0016 (17)
N3_10.022 (3)0.033 (4)0.031 (3)0.008 (3)0.014 (2)0.005 (3)
O19_10.038 (4)0.032 (5)0.042 (5)0.007 (4)0.021 (4)0.010 (3)
O20_10.026 (9)0.034 (9)0.030 (3)0.007 (5)0.006 (3)0.002 (3)
O21_10.043 (4)0.040 (5)0.038 (5)0.017 (4)0.012 (4)0.014 (3)
N3'_10.022 (3)0.033 (4)0.031 (3)0.008 (3)0.014 (2)0.005 (3)
O19'_10.038 (4)0.032 (5)0.042 (5)0.007 (4)0.021 (4)0.010 (3)
O20'_10.026 (9)0.034 (9)0.030 (3)0.007 (5)0.006 (3)0.002 (3)
O21'_10.043 (4)0.040 (5)0.038 (5)0.017 (4)0.012 (4)0.014 (3)
O18_10.055 (3)0.036 (2)0.037 (2)0.006 (2)0.020 (2)0.008 (2)
C1_20.031 (3)0.033 (3)0.025 (3)0.000 (2)0.015 (3)0.005 (2)
C2_20.031 (3)0.037 (3)0.027 (3)0.001 (2)0.018 (3)0.006 (2)
C3_20.042 (3)0.037 (3)0.030 (3)0.001 (3)0.024 (3)0.010 (3)
C4_20.031 (3)0.036 (3)0.026 (3)0.002 (2)0.015 (3)0.007 (2)
C5_20.029 (3)0.016 (3)0.045 (3)0.001 (2)0.024 (3)0.000 (2)
C6_20.028 (3)0.026 (3)0.036 (3)0.000 (2)0.020 (3)0.007 (2)
C7_20.033 (3)0.027 (3)0.027 (3)0.004 (2)0.017 (3)0.004 (2)
C8_20.021 (3)0.034 (3)0.024 (3)0.002 (2)0.011 (2)0.002 (2)
C9_20.027 (3)0.024 (3)0.035 (3)0.004 (2)0.021 (3)0.001 (2)
C10_20.034 (3)0.019 (3)0.033 (3)0.002 (2)0.022 (3)0.001 (2)
O1_20.0283 (19)0.0258 (19)0.024 (2)0.0013 (15)0.0152 (17)0.0005 (15)
O2_20.033 (2)0.0260 (19)0.027 (2)0.0002 (15)0.0177 (18)0.0005 (15)
O3_20.031 (2)0.0227 (18)0.031 (2)0.0039 (15)0.0186 (18)0.0019 (15)
O4_20.035 (2)0.0260 (19)0.031 (2)0.0013 (16)0.0218 (18)0.0008 (16)
O5_20.0185 (18)0.0198 (17)0.0245 (19)0.0026 (14)0.0094 (16)0.0003 (15)
Ni2_20.0186 (3)0.0166 (3)0.0229 (4)0.0010 (2)0.0129 (3)0.0004 (3)
O6_20.0187 (18)0.0294 (19)0.026 (2)0.0039 (15)0.0143 (16)0.0054 (16)
O7_20.0160 (18)0.0243 (19)0.027 (2)0.0036 (14)0.0133 (17)0.0055 (15)
O8_20.030 (2)0.030 (2)0.025 (2)0.0002 (16)0.0135 (18)0.0049 (16)
O9_20.0237 (19)0.0182 (18)0.033 (2)0.0011 (15)0.0152 (17)0.0070 (15)
O10_20.027 (2)0.0207 (19)0.028 (2)0.0067 (15)0.0118 (18)0.0016 (16)
O11_20.0255 (19)0.0184 (18)0.026 (2)0.0005 (14)0.0131 (17)0.0031 (15)
N1_20.027 (2)0.020 (2)0.024 (3)0.0014 (19)0.015 (2)0.0003 (19)
O12_20.0251 (19)0.0223 (18)0.026 (2)0.0012 (15)0.0124 (17)0.0036 (16)
O13_20.030 (2)0.0252 (19)0.033 (2)0.0101 (16)0.0103 (19)0.0044 (16)
O14_20.046 (2)0.024 (2)0.032 (2)0.0139 (17)0.025 (2)0.0023 (16)
N2_20.030 (3)0.025 (2)0.027 (3)0.001 (2)0.016 (2)0.002 (2)
O15_20.036 (2)0.031 (2)0.055 (3)0.0017 (17)0.027 (2)0.0195 (19)
O16_20.0266 (19)0.0237 (18)0.028 (2)0.0083 (15)0.0147 (17)0.0041 (16)
O17_20.017 (2)0.045 (2)0.041 (2)0.0058 (17)0.0093 (18)0.0058 (18)
O18_20.047 (2)0.029 (2)0.038 (2)0.0062 (18)0.026 (2)0.0077 (18)
C1_30.021 (3)0.030 (3)0.022 (3)0.003 (2)0.010 (2)0.001 (2)
C2_30.029 (3)0.027 (3)0.021 (3)0.001 (2)0.011 (2)0.003 (2)
C3_30.029 (3)0.017 (3)0.036 (3)0.004 (2)0.018 (3)0.005 (2)
C4_30.026 (3)0.022 (3)0.041 (3)0.002 (2)0.021 (3)0.002 (2)
C5_30.037 (3)0.028 (3)0.038 (3)0.008 (2)0.027 (3)0.010 (2)
C6_30.028 (3)0.027 (3)0.031 (3)0.008 (2)0.015 (3)0.010 (2)
C7_30.022 (3)0.030 (3)0.021 (3)0.007 (2)0.014 (2)0.005 (2)
C8_30.026 (3)0.023 (3)0.030 (3)0.002 (2)0.020 (3)0.004 (2)
C9_30.026 (3)0.028 (3)0.029 (3)0.007 (2)0.016 (3)0.004 (2)
C10_30.031 (3)0.021 (3)0.028 (3)0.002 (2)0.018 (3)0.002 (2)
O1_30.0233 (19)0.0209 (18)0.029 (2)0.0029 (14)0.0113 (17)0.0013 (15)
O2_30.0288 (19)0.0169 (17)0.035 (2)0.0000 (14)0.0219 (18)0.0006 (15)
O3_30.028 (2)0.0275 (19)0.031 (2)0.0003 (15)0.0199 (18)0.0033 (16)
O4_30.0269 (19)0.0227 (18)0.028 (2)0.0014 (15)0.0136 (17)0.0028 (15)
O5_30.0201 (18)0.0309 (19)0.0225 (19)0.0036 (15)0.0128 (16)0.0028 (15)
Ni3_30.0146 (4)0.0162 (4)0.0201 (5)0.0018 (3)0.0097 (4)0.0000 (4)
O6_30.0145 (18)0.0251 (19)0.031 (2)0.0024 (14)0.0146 (17)0.0092 (15)
O8_30.026 (2)0.0155 (17)0.033 (2)0.0009 (14)0.0204 (18)0.0018 (15)
O9_30.0204 (18)0.0180 (17)0.0221 (19)0.0012 (14)0.0098 (16)0.0016 (15)
Ni4_30.0175 (5)0.0165 (4)0.0210 (5)0.0018 (3)0.0115 (4)0.0009 (4)
O7_30.0194 (18)0.0226 (18)0.033 (2)0.0024 (15)0.0176 (17)0.0051 (16)
O10_30.034 (2)0.033 (2)0.024 (2)0.0105 (17)0.0072 (19)0.0079 (17)
O11_30.029 (2)0.0163 (17)0.028 (2)0.0019 (15)0.0157 (18)0.0030 (15)
N1_30.029 (3)0.028 (2)0.020 (2)0.005 (2)0.017 (2)0.006 (2)
O12_30.028 (2)0.0208 (19)0.032 (2)0.0005 (15)0.0144 (18)0.0022 (16)
O13_30.031 (2)0.028 (2)0.030 (2)0.0113 (17)0.0093 (18)0.0040 (17)
O14_30.0218 (19)0.0247 (18)0.024 (2)0.0046 (15)0.0084 (17)0.0028 (15)
O18_30.031 (2)0.025 (2)0.027 (2)0.0009 (16)0.0146 (18)0.0004 (16)
Geometric parameters (Å, º) top
C1_1—O1_11.424 (6)C9_2—C10_21.487 (7)
C1_1—C2_11.503 (7)C9_2—H9A_20.9900
C1_1—H1A_10.9900C9_2—H9B_20.9900
C1_1—H1B_10.9900C10_2—O1_21.416 (5)
C2_1—O2_11.433 (6)C10_2—H10A_20.9900
C2_1—H2A_10.9900C10_2—H10B_20.9900
C2_1—H2B_10.9900Ni2_2—O11_22.027 (3)
C3_1—O2_11.432 (6)Ni2_2—O7_22.027 (3)
C3_1—C4_11.488 (7)Ni2_2—O9_22.040 (3)
C3_1—H3A_10.9900Ni2_2—O10_22.041 (3)
C3_1—H3B_10.9900Ni2_2—O6_22.051 (3)
C4_1—O3_11.433 (6)Ni2_2—O8_22.066 (3)
C4_1—H4A_10.9900O6_2—H6C_20.848 (19)
C4_1—H4B_10.9900O6_2—H6D_20.846 (18)
C5_1—O3_11.429 (6)O7_2—H7C_20.833 (18)
C5_1—C6_11.499 (7)O7_2—H7D_20.835 (18)
C5_1—H5A_10.9900O8_2—H8C_20.812 (19)
C5_1—H5B_10.9900O8_2—H8D_20.822 (19)
C6_1—O4_11.435 (5)O9_2—H9C_20.849 (19)
C6_1—H6A_10.9900O9_2—H9D_20.836 (19)
C6_1—H6B_10.9900O10_2—H10C_20.821 (19)
C7_1—O4_11.425 (5)O10_2—H10D_20.837 (19)
C7_1—C8_11.504 (6)O11_2—H11C_20.843 (19)
C7_1—H7A_10.9900O11_2—H11D_20.835 (18)
C7_1—H7B_10.9900N1_2—O12_21.249 (5)
C8_1—O5_11.424 (6)N1_2—O14_21.250 (5)
C8_1—H8A_10.9900N1_2—O13_21.258 (5)
C8_1—H8B_10.9900N2_2—O17_21.244 (5)
C9_1—O5_11.429 (5)N2_2—O16_21.255 (5)
C9_1—C10_11.498 (7)N2_2—O15_21.260 (5)
C9_1—H9A_10.9900O18_2—H18C_20.838 (10)
C9_1—H9B_10.9900O18_2—H18D_20.837 (10)
C10_1—O1_11.422 (5)C1_3—O1_31.428 (5)
C10_1—H10A_10.9900C1_3—C2_31.497 (6)
C10_1—H10B_10.9900C1_3—H1A_30.9900
Ni1_1—O11_12.032 (3)C1_3—H1B_30.9900
Ni1_1—O6_12.033 (3)C2_3—O2_31.438 (5)
Ni1_1—O7_12.043 (3)C2_3—H2A_30.9900
Ni1_1—O8_12.049 (4)C2_3—H2B_30.9900
Ni1_1—O10_12.059 (4)C3_3—O2_31.431 (5)
Ni1_1—O9_12.060 (4)C3_3—C4_31.481 (7)
O6_1—H6C_10.840 (19)C3_3—H3A_30.9900
O6_1—H6D_10.825 (18)C3_3—H3B_30.9900
O7_1—H7C_10.829 (18)C4_3—O3_31.434 (6)
O7_1—H7D_10.834 (18)C4_3—H4A_30.9900
O8_1—H8C_10.851 (19)C4_3—H4B_30.9900
O8_1—H8D_10.834 (19)C5_3—O3_31.426 (6)
O9_1—H9C_10.824 (19)C5_3—C6_31.507 (7)
O9_1—H9D_10.851 (19)C5_3—H5A_30.9900
O10_1—H10C_10.836 (19)C5_3—H5B_30.9900
O10_1—H10D_10.839 (19)C6_3—O4_31.425 (5)
O11_1—H11C_10.839 (19)C6_3—H6A_30.9900
O11_1—H11D_10.843 (19)C6_3—H6B_30.9900
N1_1—O14_11.241 (5)C7_3—O4_31.425 (5)
N1_1—O13_11.254 (5)C7_3—C8_31.501 (7)
N1_1—O12_11.266 (5)C7_3—H7A_30.9900
N2_1—O15_11.243 (5)C7_3—H7B_30.9900
N2_1—O16_11.250 (5)C8_3—O5_31.423 (5)
N2_1—O17_11.258 (5)C8_3—H8A_30.9900
N3_1—O20_11.240 (8)C8_3—H8B_30.9900
N3_1—O19_11.249 (8)C9_3—O5_31.448 (6)
N3_1—O21_11.254 (8)C9_3—C10_31.490 (6)
N3'_1—O20'_11.242 (8)C9_3—H9A_30.9900
N3'_1—O19'_11.250 (8)C9_3—H9B_30.9900
N3'_1—O21'_11.257 (8)C10_3—O1_31.438 (5)
O18_1—H18C_10.845 (10)C10_3—H10A_30.9900
O18_1—H18D_10.844 (10)C10_3—H10B_30.9900
C1_2—O1_21.420 (6)Ni3_3—O6_3i2.023 (3)
C1_2—C2_21.495 (7)Ni3_3—O6_32.023 (3)
C1_2—H1A_20.9900Ni3_3—O9_3i2.039 (3)
C1_2—H1B_20.9900Ni3_3—O9_32.039 (3)
C2_2—O2_21.428 (5)Ni3_3—O8_32.063 (3)
C2_2—H2A_20.9900Ni3_3—O8_3i2.063 (3)
C2_2—H2B_20.9900O6_3—H6C_30.835 (18)
C3_2—O2_21.435 (6)O6_3—H6D_30.812 (18)
C3_2—C4_21.494 (7)O8_3—H8C_30.835 (18)
C3_2—H3A_20.9900O8_3—H8D_30.836 (18)
C3_2—H3B_20.9900O9_3—H9C_30.845 (18)
C4_2—O3_21.432 (6)O9_3—H9D_30.831 (18)
C4_2—H4A_20.9900Ni4_3—O10_32.018 (3)
C4_2—H4B_20.9900Ni4_3—O10_3ii2.019 (3)
C5_2—O3_21.423 (6)Ni4_3—O7_3ii2.054 (3)
C5_2—C6_21.508 (7)Ni4_3—O7_32.054 (3)
C5_2—H5A_20.9900Ni4_3—O11_3ii2.066 (3)
C5_2—H5B_20.9900Ni4_3—O11_32.066 (3)
C6_2—O4_21.431 (5)O7_3—H7C_30.837 (18)
C6_2—H6A_20.9900O7_3—H7D_30.837 (18)
C6_2—H6B_20.9900O10_3—H10C_30.840 (19)
C7_2—O4_21.424 (6)O10_3—H10D_30.838 (19)
C7_2—C8_21.496 (6)O11_3—H11C_30.833 (18)
C7_2—H7A_20.9900O11_3—H11D_30.834 (18)
C7_2—H7B_20.9900N1_3—O13_31.244 (5)
C8_2—O5_21.422 (6)N1_3—O12_31.253 (5)
C8_2—H8A_20.9900N1_3—O14_31.271 (5)
C8_2—H8B_20.9900O18_3—H18C_30.833 (10)
C9_2—O5_21.431 (5)O18_3—H18D_30.828 (10)
O1_1—C1_1—C2_1108.4 (4)C9_2—C10_2—H10A_2109.9
O1_1—C1_1—H1A_1110.0O1_2—C10_2—H10B_2109.9
C2_1—C1_1—H1A_1110.0C9_2—C10_2—H10B_2109.9
O1_1—C1_1—H1B_1110.0H10A_2—C10_2—H10B_2108.3
C2_1—C1_1—H1B_1110.0C10_2—O1_2—C1_2115.0 (4)
H1A_1—C1_1—H1B_1108.4C2_2—O2_2—C3_2111.3 (4)
O2_1—C2_1—C1_1108.2 (4)C5_2—O3_2—C4_2114.4 (4)
O2_1—C2_1—H2A_1110.1C7_2—O4_2—C6_2114.0 (4)
C1_1—C2_1—H2A_1110.1C8_2—O5_2—C9_2114.4 (3)
O2_1—C2_1—H2B_1110.1O11_2—Ni2_2—O7_290.87 (13)
C1_1—C2_1—H2B_1110.1O11_2—Ni2_2—O9_2174.99 (14)
H2A_1—C2_1—H2B_1108.4O7_2—Ni2_2—O9_286.88 (13)
O2_1—C3_1—C4_1113.2 (4)O11_2—Ni2_2—O10_286.91 (13)
O2_1—C3_1—H3A_1108.9O7_2—Ni2_2—O10_290.25 (14)
C4_1—C3_1—H3A_1108.9O9_2—Ni2_2—O10_288.62 (14)
O2_1—C3_1—H3B_1108.9O11_2—Ni2_2—O6_291.18 (13)
C4_1—C3_1—H3B_1108.9O7_2—Ni2_2—O6_2177.34 (14)
H3A_1—C3_1—H3B_1107.7O9_2—Ni2_2—O6_291.21 (13)
O3_1—C4_1—C3_1109.1 (4)O10_2—Ni2_2—O6_291.55 (14)
O3_1—C4_1—H4A_1109.9O11_2—Ni2_2—O8_293.09 (14)
C3_1—C4_1—H4A_1109.9O7_2—Ni2_2—O8_289.51 (14)
O3_1—C4_1—H4B_1109.9O9_2—Ni2_2—O8_291.37 (14)
C3_1—C4_1—H4B_1109.9O10_2—Ni2_2—O8_2179.76 (15)
H4A_1—C4_1—H4B_1108.3O6_2—Ni2_2—O8_288.68 (14)
O3_1—C5_1—C6_1109.1 (4)Ni2_2—O6_2—H6C_2130 (3)
O3_1—C5_1—H5A_1109.9Ni2_2—O6_2—H6D_2124 (3)
C6_1—C5_1—H5A_1109.9H6C_2—O6_2—H6D_2101 (3)
O3_1—C5_1—H5B_1109.9Ni2_2—O7_2—H7C_2115 (3)
C6_1—C5_1—H5B_1109.9Ni2_2—O7_2—H7D_2127 (3)
H5A_1—C5_1—H5B_1108.3H7C_2—O7_2—H7D_2104 (3)
O4_1—C6_1—C5_1107.8 (4)Ni2_2—O8_2—H8C_2116 (3)
O4_1—C6_1—H6A_1110.2Ni2_2—O8_2—H8D_2129 (3)
C5_1—C6_1—H6A_1110.2H8C_2—O8_2—H8D_2110 (3)
O4_1—C6_1—H6B_1110.2Ni2_2—O9_2—H9C_2120 (3)
C5_1—C6_1—H6B_1110.2Ni2_2—O9_2—H9D_2114 (3)
H6A_1—C6_1—H6B_1108.5H9C_2—O9_2—H9D_2103 (3)
O4_1—C7_1—C8_1107.7 (4)Ni2_2—O10_2—H10C_2123 (3)
O4_1—C7_1—H7A_1110.2Ni2_2—O10_2—H10D_2129 (3)
C8_1—C7_1—H7A_1110.2H10C_2—O10_2—H10D_2107 (3)
O4_1—C7_1—H7B_1110.2Ni2_2—O11_2—H11C_2125 (3)
C8_1—C7_1—H7B_1110.2Ni2_2—O11_2—H11D_2106 (3)
H7A_1—C7_1—H7B_1108.5H11C_2—O11_2—H11D_2105 (3)
O5_1—C8_1—C7_1108.5 (4)O12_2—N1_2—O14_2121.7 (4)
O5_1—C8_1—H8A_1110.0O12_2—N1_2—O13_2119.5 (4)
C7_1—C8_1—H8A_1110.0O14_2—N1_2—O13_2118.8 (4)
O5_1—C8_1—H8B_1110.0O17_2—N2_2—O16_2121.4 (4)
C7_1—C8_1—H8B_1110.0O17_2—N2_2—O15_2119.7 (4)
H8A_1—C8_1—H8B_1108.4O16_2—N2_2—O15_2119.0 (4)
O5_1—C9_1—C10_1108.5 (4)H18C_2—O18_2—H18D_2104.2 (16)
O5_1—C9_1—H9A_1110.0O1_3—C1_3—C2_3108.8 (4)
C10_1—C9_1—H9A_1110.0O1_3—C1_3—H1A_3109.9
O5_1—C9_1—H9B_1110.0C2_3—C1_3—H1A_3109.9
C10_1—C9_1—H9B_1110.0O1_3—C1_3—H1B_3109.9
H9A_1—C9_1—H9B_1108.4C2_3—C1_3—H1B_3109.9
O1_1—C10_1—C9_1107.7 (4)H1A_3—C1_3—H1B_3108.3
O1_1—C10_1—H10A_1110.2O2_3—C2_3—C1_3108.0 (4)
C9_1—C10_1—H10A_1110.2O2_3—C2_3—H2A_3110.1
O1_1—C10_1—H10B_1110.2C1_3—C2_3—H2A_3110.1
C9_1—C10_1—H10B_1110.2O2_3—C2_3—H2B_3110.1
H10A_1—C10_1—H10B_1108.5C1_3—C2_3—H2B_3110.1
C10_1—O1_1—C1_1114.0 (4)H2A_3—C2_3—H2B_3108.4
C3_1—O2_1—C2_1113.7 (4)O2_3—C3_3—C4_3108.8 (4)
C5_1—O3_1—C4_1112.4 (3)O2_3—C3_3—H3A_3109.9
C7_1—O4_1—C6_1114.5 (3)C4_3—C3_3—H3A_3109.9
C8_1—O5_1—C9_1114.1 (3)O2_3—C3_3—H3B_3109.9
O11_1—Ni1_1—O6_194.46 (13)C4_3—C3_3—H3B_3109.9
O11_1—Ni1_1—O7_188.51 (13)H3A_3—C3_3—H3B_3108.3
O6_1—Ni1_1—O7_1174.74 (14)O3_3—C4_3—C3_3108.6 (4)
O11_1—Ni1_1—O8_189.76 (16)O3_3—C4_3—H4A_3110.0
O6_1—Ni1_1—O8_190.13 (14)C3_3—C4_3—H4A_3110.0
O7_1—Ni1_1—O8_185.54 (14)O3_3—C4_3—H4B_3110.0
O11_1—Ni1_1—O10_187.76 (14)C3_3—C4_3—H4B_3110.0
O6_1—Ni1_1—O10_189.34 (14)H4A_3—C4_3—H4B_3108.4
O7_1—Ni1_1—O10_195.11 (14)O3_3—C5_3—C6_3107.7 (4)
O8_1—Ni1_1—O10_1177.42 (16)O3_3—C5_3—H5A_3110.2
O11_1—Ni1_1—O9_1177.02 (17)C6_3—C5_3—H5A_3110.2
O6_1—Ni1_1—O9_187.01 (15)O3_3—C5_3—H5B_3110.2
O7_1—Ni1_1—O9_190.22 (15)C6_3—C5_3—H5B_3110.2
O8_1—Ni1_1—O9_192.8 (2)H5A_3—C5_3—H5B_3108.5
O10_1—Ni1_1—O9_189.67 (19)O4_3—C6_3—C5_3107.4 (4)
Ni1_1—O6_1—H6C_1120 (3)O4_3—C6_3—H6A_3110.2
Ni1_1—O6_1—H6D_1128 (3)C5_3—C6_3—H6A_3110.2
H6C_1—O6_1—H6D_1106 (3)O4_3—C6_3—H6B_3110.2
Ni1_1—O7_1—H7C_1119 (3)C5_3—C6_3—H6B_3110.2
Ni1_1—O7_1—H7D_1128 (3)H6A_3—C6_3—H6B_3108.5
H7C_1—O7_1—H7D_1106 (3)O4_3—C7_3—C8_3107.9 (4)
Ni1_1—O8_1—H8C_1117 (4)O4_3—C7_3—H7A_3110.1
Ni1_1—O8_1—H8D_1126 (4)C8_3—C7_3—H7A_3110.1
H8C_1—O8_1—H8D_1104 (3)O4_3—C7_3—H7B_3110.1
Ni1_1—O9_1—H9C_1123 (5)C8_3—C7_3—H7B_3110.1
Ni1_1—O9_1—H9D_1105 (5)H7A_3—C7_3—H7B_3108.4
H9C_1—O9_1—H9D_1104 (3)O5_3—C8_3—C7_3108.8 (4)
Ni1_1—O10_1—H10C_1113 (4)O5_3—C8_3—H8A_3109.9
Ni1_1—O10_1—H10D_1117 (4)C7_3—C8_3—H8A_3109.9
H10C_1—O10_1—H10D_1105 (3)O5_3—C8_3—H8B_3109.9
Ni1_1—O11_1—H11C_1125 (3)C7_3—C8_3—H8B_3109.9
Ni1_1—O11_1—H11D_1125 (3)H8A_3—C8_3—H8B_3108.3
H11C_1—O11_1—H11D_1104 (3)O5_3—C9_3—C10_3107.7 (4)
O14_1—N1_1—O13_1120.2 (4)O5_3—C9_3—H9A_3110.2
O14_1—N1_1—O12_1119.7 (5)C10_3—C9_3—H9A_3110.2
O13_1—N1_1—O12_1120.0 (4)O5_3—C9_3—H9B_3110.2
O15_1—N2_1—O16_1119.4 (4)C10_3—C9_3—H9B_3110.2
O15_1—N2_1—O17_1120.9 (4)H9A_3—C9_3—H9B_3108.5
O16_1—N2_1—O17_1119.7 (4)O1_3—C10_3—C9_3112.5 (4)
O20_1—N3_1—O19_1119.6 (9)O1_3—C10_3—H10A_3109.1
O20_1—N3_1—O21_1120.7 (9)C9_3—C10_3—H10A_3109.1
O19_1—N3_1—O21_1119.7 (9)O1_3—C10_3—H10B_3109.1
O20'_1—N3'_1—O19'_1119.4 (10)C9_3—C10_3—H10B_3109.1
O20'_1—N3'_1—O21'_1120.4 (10)H10A_3—C10_3—H10B_3107.8
O19'_1—N3'_1—O21'_1120.3 (10)C1_3—O1_3—C10_3114.1 (3)
H18C_1—O18_1—H18D_1102.4 (16)C3_3—O2_3—C2_3112.9 (3)
O1_2—C1_2—C2_2108.1 (4)C5_3—O3_3—C4_3114.8 (3)
O1_2—C1_2—H1A_2110.1C7_3—O4_3—C6_3113.2 (4)
C2_2—C1_2—H1A_2110.1C8_3—O5_3—C9_3113.8 (3)
O1_2—C1_2—H1B_2110.1O6_3i—Ni3_3—O6_3180.0
C2_2—C1_2—H1B_2110.1O6_3i—Ni3_3—O9_3i90.79 (13)
H1A_2—C1_2—H1B_2108.4O6_3—Ni3_3—O9_3i89.21 (13)
O2_2—C2_2—C1_2108.5 (4)O6_3i—Ni3_3—O9_389.21 (13)
O2_2—C2_2—H2A_2110.0O6_3—Ni3_3—O9_390.79 (13)
C1_2—C2_2—H2A_2110.0O9_3i—Ni3_3—O9_3180.0
O2_2—C2_2—H2B_2110.0O6_3i—Ni3_3—O8_388.78 (13)
C1_2—C2_2—H2B_2110.0O6_3—Ni3_3—O8_391.23 (13)
H2A_2—C2_2—H2B_2108.4O9_3i—Ni3_3—O8_386.11 (13)
O2_2—C3_2—C4_2108.0 (4)O9_3—Ni3_3—O8_393.89 (13)
O2_2—C3_2—H3A_2110.1O6_3i—Ni3_3—O8_3i91.22 (13)
C4_2—C3_2—H3A_2110.1O6_3—Ni3_3—O8_3i88.77 (13)
O2_2—C3_2—H3B_2110.1O9_3i—Ni3_3—O8_3i93.89 (13)
C4_2—C3_2—H3B_2110.1O9_3—Ni3_3—O8_3i86.11 (13)
H3A_2—C3_2—H3B_2108.4O8_3—Ni3_3—O8_3i180.0
O3_2—C4_2—C3_2112.1 (4)Ni3_3—O6_3—H6C_3116 (3)
O3_2—C4_2—H4A_2109.2Ni3_3—O6_3—H6D_3130 (3)
C3_2—C4_2—H4A_2109.2H6C_3—O6_3—H6D_3107 (3)
O3_2—C4_2—H4B_2109.2Ni3_3—O8_3—H8C_3117 (3)
C3_2—C4_2—H4B_2109.2Ni3_3—O8_3—H8D_3131 (3)
H4A_2—C4_2—H4B_2107.9H8C_3—O8_3—H8D_3105 (3)
O3_2—C5_2—C6_2108.8 (4)Ni3_3—O9_3—H9C_3118 (3)
O3_2—C5_2—H5A_2109.9Ni3_3—O9_3—H9D_3113 (3)
C6_2—C5_2—H5A_2109.9H9C_3—O9_3—H9D_3104 (3)
O3_2—C5_2—H5B_2109.9O10_3—Ni4_3—O10_3ii180.0
C6_2—C5_2—H5B_2109.9O10_3—Ni4_3—O7_3ii89.99 (15)
H5A_2—C5_2—H5B_2108.3O10_3ii—Ni4_3—O7_3ii90.02 (15)
O4_2—C6_2—C5_2107.8 (4)O10_3—Ni4_3—O7_390.01 (15)
O4_2—C6_2—H6A_2110.1O10_3ii—Ni4_3—O7_389.99 (15)
C5_2—C6_2—H6A_2110.1O7_3ii—Ni4_3—O7_3179.998 (1)
O4_2—C6_2—H6B_2110.1O10_3—Ni4_3—O11_3ii91.03 (14)
C5_2—C6_2—H6B_2110.1O10_3ii—Ni4_3—O11_3ii88.97 (14)
H6A_2—C6_2—H6B_2108.5O7_3ii—Ni4_3—O11_3ii90.36 (13)
O4_2—C7_2—C8_2107.5 (4)O7_3—Ni4_3—O11_3ii89.64 (13)
O4_2—C7_2—H7A_2110.2O10_3—Ni4_3—O11_388.97 (14)
C8_2—C7_2—H7A_2110.2O10_3ii—Ni4_3—O11_391.03 (14)
O4_2—C7_2—H7B_2110.2O7_3ii—Ni4_3—O11_389.64 (13)
C8_2—C7_2—H7B_2110.2O7_3—Ni4_3—O11_390.36 (13)
H7A_2—C7_2—H7B_2108.5O11_3ii—Ni4_3—O11_3179.999 (2)
O5_2—C8_2—C7_2108.5 (4)Ni4_3—O7_3—H7C_3118 (3)
O5_2—C8_2—H8A_2110.0Ni4_3—O7_3—H7D_3118 (3)
C7_2—C8_2—H8A_2110.0H7C_3—O7_3—H7D_3105 (3)
O5_2—C8_2—H8B_2110.0Ni4_3—O10_3—H10C_3124 (3)
C7_2—C8_2—H8B_2110.0Ni4_3—O10_3—H10D_3129 (3)
H8A_2—C8_2—H8B_2108.4H10C_3—O10_3—H10D_3104 (3)
O5_2—C9_2—C10_2108.6 (4)Ni4_3—O11_3—H11C_3122 (3)
O5_2—C9_2—H9A_2110.0Ni4_3—O11_3—H11D_3127 (3)
C10_2—C9_2—H9A_2110.0H11C_3—O11_3—H11D_3105 (3)
O5_2—C9_2—H9B_2110.0O13_3—N1_3—O12_3121.5 (4)
C10_2—C9_2—H9B_2110.0O13_3—N1_3—O14_3119.7 (4)
H9A_2—C9_2—H9B_2108.4O12_3—N1_3—O14_3118.8 (4)
O1_2—C10_2—C9_2109.0 (4)H18C_3—O18_3—H18D_3105.7 (17)
O1_2—C10_2—H10A_2109.9
O1_1—C1_1—C2_1—O2_171.7 (5)C4_2—C3_2—O2_2—C2_2176.4 (4)
O2_1—C3_1—C4_1—O3_158.0 (5)C6_2—C5_2—O3_2—C4_2170.3 (4)
O3_1—C5_1—C6_1—O4_172.2 (5)C3_2—C4_2—O3_2—C5_283.4 (5)
O4_1—C7_1—C8_1—O5_166.2 (5)C8_2—C7_2—O4_2—C6_2178.0 (4)
O5_1—C9_1—C10_1—O1_161.3 (5)C5_2—C6_2—O4_2—C7_2168.7 (4)
C9_1—C10_1—O1_1—C1_1174.4 (4)C7_2—C8_2—O5_2—C9_2163.9 (4)
C2_1—C1_1—O1_1—C10_1167.2 (4)C10_2—C9_2—O5_2—C8_2159.4 (4)
C4_1—C3_1—O2_1—C2_180.4 (5)O1_3—C1_3—C2_3—O2_376.3 (5)
C1_1—C2_1—O2_1—C3_1167.4 (4)O2_3—C3_3—C4_3—O3_365.7 (5)
C6_1—C5_1—O3_1—C4_1163.7 (4)O3_3—C5_3—C6_3—O4_362.3 (5)
C3_1—C4_1—O3_1—C5_1175.4 (4)O4_3—C7_3—C8_3—O5_373.1 (4)
C8_1—C7_1—O4_1—C6_1165.1 (4)O5_3—C9_3—C10_3—O1_360.7 (5)
C5_1—C6_1—O4_1—C7_1165.6 (4)C2_3—C1_3—O1_3—C10_3173.5 (4)
C7_1—C8_1—O5_1—C9_1160.9 (4)C9_3—C10_3—O1_3—C1_395.8 (5)
C10_1—C9_1—O5_1—C8_1163.0 (4)C4_3—C3_3—O2_3—C2_3172.0 (4)
O1_2—C1_2—C2_2—O2_267.5 (5)C1_3—C2_3—O2_3—C3_3166.1 (4)
O2_2—C3_2—C4_2—O3_259.0 (6)C6_3—C5_3—O3_3—C4_3161.5 (4)
O3_2—C5_2—C6_2—O4_275.1 (5)C3_3—C4_3—O3_3—C5_3160.1 (4)
O4_2—C7_2—C8_2—O5_260.8 (5)C8_3—C7_3—O4_3—C6_3179.2 (4)
O5_2—C9_2—C10_2—O1_264.6 (5)C5_3—C6_3—O4_3—C7_3176.4 (4)
C9_2—C10_2—O1_2—C1_2173.0 (4)C7_3—C8_3—O5_3—C9_3150.4 (4)
C2_2—C1_2—O1_2—C10_2166.7 (4)C10_3—C9_3—O5_3—C8_3172.5 (4)
C1_2—C2_2—O2_2—C3_2160.8 (4)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6_1—H6C_1···O3_10.84 (2)1.97 (2)2.792 (4)167 (5)
O6_1—H6D_1···O5_10.83 (2)1.96 (2)2.767 (4)165 (5)
O7_1—H7C_1···O1_2iii0.83 (2)1.97 (2)2.797 (5)172 (5)
O7_1—H7D_1···O4_2iii0.83 (2)1.88 (2)2.711 (4)173 (5)
O8_1—H8C_1···O2_10.85 (2)1.93 (2)2.766 (5)169 (6)
O6_2—H6D_2···O2_20.85 (2)2.03 (2)2.870 (4)175 (4)
O6_2—H6C_2···O5_20.85 (2)2.00 (2)2.815 (4)160 (5)
O7_2—H7D_2···O1_10.84 (2)1.89 (2)2.717 (4)173 (5)
O7_2—H7C_2···O4_10.83 (2)1.93 (2)2.752 (4)169 (5)
O9_2—H9D_2···O3_20.84 (2)1.93 (2)2.754 (4)167 (5)
O6_3—H6C_3···O1_30.84 (2)1.93 (2)2.753 (4)168 (5)
O6_3—H6D_3···O3_30.81 (2)1.99 (2)2.788 (4)166 (5)
O7_3—H7D_3···O2_3ii0.84 (2)1.94 (2)2.771 (4)171 (5)
O7_3—H7C_3···O4_3ii0.84 (2)1.96 (2)2.780 (5)167 (5)
O8_3—H8C_3···O5_3i0.84 (2)1.98 (2)2.810 (4)174 (5)
O8_1—H8D_1···O19_10.83 (2)1.84 (3)2.650 (9)164 (5)
O9_1—H9C_1···O20_1iv0.82 (2)2.32 (6)2.887 (14)126 (5)
O9_1—H9C_1···O20_10.82 (2)2.14 (4)2.771 (12)134 (6)
O10_1—H10C_1···O12_10.84 (2)2.10 (3)2.867 (5)151 (4)
O10_1—H10D_1···O17_10.84 (2)1.93 (2)2.745 (5)164 (5)
O11_1—H11D_1···O15_10.84 (2)1.91 (2)2.746 (5)176 (5)
O11_1—H11C_1···O18_10.84 (2)1.86 (2)2.690 (5)168 (5)
O8_2—H8C_2···O12_1v0.81 (2)2.03 (2)2.834 (5)170 (5)
O9_2—H9C_2···O13_1v0.85 (2)1.96 (2)2.797 (5)168 (5)
O10_2—H10C_2···O14_20.82 (2)2.03 (2)2.838 (5)169 (4)
O10_2—H10D_2···O18_20.84 (2)1.92 (2)2.727 (5)161 (5)
O11_2—H11C_2···O12_20.84 (2)1.91 (2)2.746 (5)174 (4)
O11_2—H11D_2···O15_20.84 (2)1.92 (3)2.693 (5)154 (5)
O8_3—H8D_3···O13_2vi0.84 (2)1.94 (2)2.770 (4)174 (4)
O9_3—H9C_3···O14_3i0.85 (2)1.94 (2)2.777 (4)171 (5)
O9_3—H9D_3···O18_3i0.83 (2)1.96 (2)2.764 (5)161 (4)
O10_3—H10C_3···O12_3v0.84 (2)1.87 (2)2.702 (5)168 (6)
O10_3—H10D_3···O16_2ii0.84 (2)1.86 (2)2.669 (5)163 (5)
O11_3—H11C_3···O13_3v0.83 (2)1.99 (2)2.822 (5)175 (5)
O11_3—H11D_3···O16_1v0.83 (2)2.02 (2)2.848 (5)176 (5)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z; (iii) x1, y, z; (iv) x, y+1, z+1; (v) x, y, z1; (vi) x+1, y, z+1.
(3) top
Crystal data top
C10H20O5·C2H16NiO6·2(NO3)·C10H20O5·H12NiO6·2(NO3)F(000) = 1112
Mr = 1050.22Dx = 1.548 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 5368 reflections
a = 16.241 (1) Åθ = 1.0–27.5°
b = 15.481 (1) ŵ = 0.94 mm1
c = 10.429 (1) ÅT = 90 K
β = 120.75 (1)°Irregular block, pale green
V = 2253.5 (4) Å30.20 × 0.15 × 0.11 mm
Z = 2
Data collection top
Nonius KappaCCD
diffractometer
5174 independent reflections
Radiation source: fine-focus sealed tube3430 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
Detector resolution: 18 pixels mm-1θmax = 27.5°, θmin = 2.0°
ω scans at fixed χ = 55°h = 2121
Absorption correction: multi-scan
Scalepack (Otwinowski & Minor, 2006)
k = 2020
Tmin = 0.834, Tmax = 0.903l = 1313
10144 measured reflections
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)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.101H atoms treated by a mixture of independent and constrained refinement
S = 1.03 w = 1/[σ2(Fo2) + (0.0536P)2]
where P = (Fo2 + 2Fc2)/3
5174 reflections(Δ/σ)max < 0.001
348 parametersΔρmax = 0.71 e Å3
51 restraintsΔρmin = 0.51 e Å3
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
C10.2556 (5)0.1809 (4)0.0093 (5)0.0224 (11)0.575 (3)
H1A0.20800.20760.01100.027*0.575 (3)
H1B0.30470.22470.00820.027*0.575 (3)
C20.2074 (7)0.1493 (5)0.1673 (6)0.0222 (12)0.575 (3)
H2A0.25410.11870.18530.027*0.575 (3)
H2B0.18080.19860.23730.027*0.575 (3)
C30.0934 (4)0.0406 (5)0.3240 (9)0.0290 (14)0.575 (3)
H3A0.02730.02410.35230.035*0.575 (3)
H3B0.08860.07790.40460.035*0.575 (3)
C100.3189 (4)0.1213 (4)0.2342 (5)0.0301 (12)0.575 (3)
H10A0.35670.17470.27690.036*0.575 (3)
H10B0.25840.12640.23510.036*0.575 (3)
O10.29969 (19)0.10765 (17)0.0869 (3)0.0243 (8)0.575 (3)
O20.13244 (19)0.09210 (16)0.1901 (3)0.0212 (7)0.575 (3)
C1'0.2800 (7)0.1722 (7)0.0399 (8)0.0224 (11)0.425 (3)
H1'10.29320.23430.06430.027*0.425 (3)
H1'20.34150.14250.07100.027*0.425 (3)
C2'0.2121 (10)0.1605 (6)0.1250 (9)0.0222 (12)0.425 (3)
H2'10.23530.19330.18190.027*0.425 (3)
H2'20.14780.18250.15300.027*0.425 (3)
C3'0.1222 (7)0.0493 (6)0.3006 (12)0.0290 (14)0.425 (3)
H3'10.06340.05190.29450.035*0.425 (3)
H3'20.11520.08780.38130.035*0.425 (3)
C10'0.3005 (5)0.1207 (5)0.2723 (7)0.0301 (12)0.425 (3)
H10C0.33710.17460.31560.036*0.425 (3)
H10D0.26170.11070.31950.036*0.425 (3)
O1'0.2353 (2)0.1356 (2)0.1156 (4)0.0206 (10)0.425 (3)
O2'0.2069 (3)0.0695 (2)0.1594 (4)0.0233 (10)0.425 (3)
C40.14547 (18)0.03982 (17)0.3203 (3)0.0309 (6)
H4A0.21130.02530.29570.037*
H4B0.11200.06810.41940.037*
C50.19807 (16)0.17591 (15)0.1985 (2)0.0229 (5)
H5A0.15610.21500.28190.028*
H5B0.25630.16390.20330.028*
C60.22495 (15)0.21744 (15)0.0523 (2)0.0207 (5)
H6A0.24950.27660.04770.025*
H6B0.16830.22120.04050.025*
C70.31257 (15)0.18047 (14)0.2085 (2)0.0183 (5)
H7A0.25050.18240.20500.022*
H7B0.34560.23640.24760.022*
C80.37293 (15)0.10806 (14)0.3069 (2)0.0211 (5)
H8A0.43130.10150.30020.025*
H8B0.39280.12040.41200.025*
C90.37305 (16)0.04593 (15)0.3188 (3)0.0264 (6)
H9A0.39100.05240.42440.032*
H9B0.43260.04130.31530.032*
O30.14881 (10)0.09710 (10)0.21010 (16)0.0210 (4)
O40.29728 (10)0.16516 (9)0.06293 (15)0.0178 (3)
O50.31728 (10)0.03030 (10)0.25838 (16)0.0211 (4)
Ni10.50000.00000.00000.01354 (11)
O70.62612 (11)0.02569 (11)0.00679 (19)0.0242 (4)
H7C0.6421 (17)0.0696 (11)0.022 (3)0.036*
H7D0.6614 (16)0.0121 (12)0.017 (3)0.036*
O80.42130 (12)0.07295 (11)0.18908 (17)0.0248 (4)
H8C0.3871 (15)0.0493 (14)0.271 (2)0.037*
H8D0.4431 (17)0.1166 (12)0.203 (3)0.037*
O90.51406 (11)0.10859 (10)0.12079 (17)0.0200 (3)
H9C0.5175 (16)0.1557 (12)0.084 (2)0.030*
H9D0.5602 (14)0.1092 (14)0.2100 (17)0.030*
Ni20.00000.00000.00000.01295 (11)
O60.12290 (10)0.05293 (10)0.02445 (17)0.0183 (3)
H6C0.1270 (15)0.0663 (14)0.0502 (18)0.027*
H6D0.1757 (12)0.0367 (15)0.0895 (19)0.027*
O100.06786 (12)0.02105 (11)0.22246 (17)0.0253 (4)
H10E0.1105 (16)0.0132 (12)0.282 (2)0.038*
H10F0.0745 (17)0.0677 (11)0.263 (3)0.038*
O110.04652 (11)0.11770 (10)0.03048 (18)0.0219 (4)
H11D0.0753 (16)0.1081 (16)0.069 (3)0.033*
C110.00716 (16)0.19561 (14)0.0769 (3)0.0262 (6)
H11A0.01760.21650.00240.039*
H11B0.02820.23920.09770.039*
H11C0.06910.18490.16740.039*
N10.46460 (13)0.27268 (12)0.1179 (2)0.0210 (4)
O120.46900 (12)0.25755 (10)0.00340 (17)0.0316 (4)
O130.41547 (10)0.33478 (9)0.11782 (16)0.0247 (4)
O140.50915 (10)0.22561 (10)0.23208 (16)0.0208 (3)
N20.72821 (13)0.07374 (13)0.48854 (19)0.0209 (4)
O150.66587 (11)0.12709 (10)0.40313 (17)0.0290 (4)
O160.80361 (11)0.10068 (10)0.60019 (16)0.0241 (4)
O170.71584 (13)0.00565 (9)0.46263 (18)0.0232 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.020 (4)0.0171 (19)0.029 (3)0.0015 (19)0.013 (3)0.007 (2)
C20.0215 (16)0.019 (2)0.029 (3)0.0001 (14)0.016 (3)0.0037 (19)
C30.043 (4)0.022 (2)0.025 (3)0.014 (2)0.019 (2)0.0014 (14)
C100.035 (3)0.0221 (16)0.027 (2)0.0138 (17)0.0113 (16)0.0060 (19)
O10.0288 (17)0.0189 (16)0.0279 (15)0.0051 (13)0.0164 (13)0.0053 (12)
O20.0196 (16)0.0217 (15)0.0236 (15)0.0024 (12)0.0119 (13)0.0015 (12)
C1'0.020 (4)0.0171 (19)0.029 (3)0.0015 (19)0.013 (3)0.007 (2)
C2'0.0215 (16)0.019 (2)0.029 (3)0.0001 (14)0.016 (3)0.0037 (19)
C3'0.043 (4)0.022 (2)0.025 (3)0.014 (2)0.019 (2)0.0014 (14)
C10'0.035 (3)0.0221 (16)0.027 (2)0.0138 (17)0.0113 (16)0.0060 (19)
O1'0.0150 (19)0.021 (2)0.0244 (19)0.0022 (16)0.0090 (15)0.0005 (16)
O2'0.023 (2)0.022 (2)0.023 (2)0.0010 (17)0.0098 (17)0.0021 (15)
C40.0322 (14)0.0419 (16)0.0226 (13)0.0045 (13)0.0170 (11)0.0076 (12)
C50.0194 (12)0.0276 (14)0.0227 (12)0.0006 (10)0.0115 (10)0.0065 (10)
C60.0176 (11)0.0173 (12)0.0251 (12)0.0036 (10)0.0093 (9)0.0061 (10)
C70.0211 (12)0.0196 (12)0.0184 (11)0.0011 (9)0.0131 (10)0.0024 (9)
C80.0181 (11)0.0246 (13)0.0208 (12)0.0039 (10)0.0101 (10)0.0002 (10)
C90.0260 (13)0.0274 (15)0.0270 (13)0.0092 (11)0.0144 (11)0.0102 (11)
O30.0203 (8)0.0260 (9)0.0185 (8)0.0033 (7)0.0113 (7)0.0032 (7)
O40.0170 (8)0.0189 (8)0.0173 (8)0.0036 (6)0.0086 (7)0.0020 (6)
O50.0198 (8)0.0168 (8)0.0246 (9)0.0030 (7)0.0100 (7)0.0033 (7)
Ni10.0131 (2)0.0132 (2)0.0144 (2)0.00119 (15)0.00712 (16)0.00089 (15)
O70.0198 (9)0.0214 (9)0.0372 (10)0.0015 (7)0.0186 (8)0.0081 (8)
O80.0276 (9)0.0199 (9)0.0184 (8)0.0059 (7)0.0057 (7)0.0032 (7)
O90.0227 (8)0.0158 (8)0.0176 (8)0.0015 (7)0.0076 (7)0.0001 (7)
Ni20.0114 (2)0.0126 (2)0.0150 (2)0.00084 (15)0.00678 (16)0.00100 (15)
O60.0152 (8)0.0226 (9)0.0174 (8)0.0021 (7)0.0085 (7)0.0022 (7)
O100.0261 (9)0.0239 (10)0.0174 (9)0.0066 (7)0.0049 (7)0.0051 (7)
O110.0199 (8)0.0184 (9)0.0326 (9)0.0004 (7)0.0170 (7)0.0012 (7)
C110.0232 (13)0.0173 (13)0.0377 (14)0.0020 (10)0.0152 (11)0.0013 (11)
N10.0210 (10)0.0145 (10)0.0251 (11)0.0020 (8)0.0100 (9)0.0029 (8)
O120.0524 (11)0.0240 (10)0.0243 (9)0.0077 (8)0.0239 (8)0.0003 (7)
O130.0244 (9)0.0154 (8)0.0326 (9)0.0025 (7)0.0133 (8)0.0048 (7)
O140.0187 (8)0.0205 (8)0.0210 (8)0.0002 (7)0.0084 (7)0.0008 (7)
N20.0242 (11)0.0222 (12)0.0173 (10)0.0014 (9)0.0112 (9)0.0007 (8)
O150.0264 (9)0.0279 (10)0.0206 (8)0.0055 (8)0.0033 (7)0.0027 (7)
O160.0196 (8)0.0264 (9)0.0177 (8)0.0026 (7)0.0033 (7)0.0026 (7)
O170.0288 (9)0.0191 (10)0.0193 (8)0.0044 (7)0.0106 (7)0.0027 (7)
Geometric parameters (Å, º) top
C1—O11.439 (6)C7—H7A0.9900
C1—C21.500 (6)C7—H7B0.9900
C1—H1A0.9900C8—O51.433 (3)
C1—H1B0.9900C8—H8A0.9900
C2—O21.423 (8)C8—H8B0.9900
C2—H2A0.9900C9—O51.424 (3)
C2—H2B0.9900C9—H9A0.9900
C3—O21.443 (6)C9—H9B0.9900
C3—C41.495 (7)Ni1—O92.0423 (15)
C3—H3A0.9900Ni1—O9i2.0423 (15)
C3—H3B0.9900Ni1—O72.0519 (15)
C10—O11.419 (5)Ni1—O7i2.0521 (15)
C10—C91.456 (5)Ni1—O82.0543 (15)
C10—H10A0.9900Ni1—O8i2.0543 (15)
C10—H10B0.9900O7—H7C0.837 (15)
C1'—O1'1.434 (10)O7—H7D0.786 (15)
C1'—C2'1.506 (8)O8—H8C0.832 (15)
C1'—H1'10.9900O8—H8D0.809 (15)
C1'—H1'20.9900O9—H9C0.838 (15)
C2'—O2'1.446 (10)O9—H9D0.845 (15)
C2'—H2'10.9900Ni2—O102.0221 (15)
C2'—H2'20.9900Ni2—O10ii2.0221 (15)
C3'—O2'1.444 (7)Ni2—O6ii2.0494 (14)
C3'—C41.472 (8)Ni2—O62.0494 (14)
C3'—H3'10.9900Ni2—O112.0586 (15)
C3'—H3'20.9900Ni2—O11ii2.0587 (15)
C10'—O1'1.441 (6)O6—H6C0.840 (15)
C10'—C91.543 (7)O6—H6D0.815 (15)
C10'—H10C0.9900O10—H10E0.839 (15)
C10'—H10D0.9900O10—H10F0.817 (15)
C4—O31.430 (3)O11—C111.420 (3)
C4—H4A0.9900O11—H11D0.773 (16)
C4—H4B0.9900C11—H11A0.9800
C5—O31.430 (3)C11—H11B0.9800
C5—C61.499 (3)C11—H11C0.9800
C5—H5A0.9900N1—O131.249 (2)
C5—H5B0.9900N1—O121.254 (2)
C6—O41.427 (2)N1—O141.262 (2)
C6—H6A0.9900N2—O171.252 (2)
C6—H6B0.9900N2—O161.253 (2)
C7—O41.427 (2)N2—O151.256 (2)
C7—C81.497 (3)
O1—C1—C2107.6 (6)O5—C8—C7108.25 (17)
O1—C1—H1A110.2O5—C8—H8A110.0
C2—C1—H1A110.2C7—C8—H8A110.0
O1—C1—H1B110.2O5—C8—H8B110.0
C2—C1—H1B110.2C7—C8—H8B110.0
H1A—C1—H1B108.5H8A—C8—H8B108.4
O2—C2—C1108.0 (5)O5—C9—C10110.2 (3)
O2—C2—H2A110.1O5—C9—C10'105.8 (4)
C1—C2—H2A110.1O5—C9—H9A109.6
O2—C2—H2B110.1C10—C9—H9A109.6
C1—C2—H2B110.1C10'—C9—H9A91.0
H2A—C2—H2B108.4O5—C9—H9B109.6
O2—C3—C4118.2 (5)C10—C9—H9B109.6
O2—C3—H3A107.8C10'—C9—H9B130.4
C4—C3—H3A107.8H9A—C9—H9B108.1
O2—C3—H3B107.8C5—O3—C4112.75 (16)
C4—C3—H3B107.8C6—O4—C7114.97 (16)
H3A—C3—H3B107.1C9—O5—C8113.35 (16)
O1—C10—C9105.5 (4)O9—Ni1—O9i179.997 (1)
O1—C10—H10A110.6O9—Ni1—O791.40 (7)
C9—C10—H10A110.6O9i—Ni1—O788.60 (7)
O1—C10—H10B110.6O9—Ni1—O7i88.60 (7)
C9—C10—H10B110.7O9i—Ni1—O7i91.39 (7)
H10A—C10—H10B108.8O7—Ni1—O7i180.0
C10—O1—C1113.1 (4)O9—Ni1—O887.60 (6)
C2—O2—C3114.9 (5)O9i—Ni1—O892.40 (6)
O1'—C1'—C2'107.4 (8)O7—Ni1—O892.68 (7)
O1'—C1'—H1'1110.2O7i—Ni1—O887.32 (7)
C2'—C1'—H1'1110.2O9—Ni1—O8i92.40 (6)
O1'—C1'—H1'2110.2O9i—Ni1—O8i87.59 (6)
C2'—C1'—H1'2110.2O7—Ni1—O8i87.32 (7)
H1'1—C1'—H1'2108.5O7i—Ni1—O8i92.67 (7)
O2'—C2'—C1'108.4 (8)O8—Ni1—O8i180.0
O2'—C2'—H2'1110.0Ni1—O7—H7C129.3 (17)
C1'—C2'—H2'1110.0Ni1—O7—H7D120.2 (18)
O2'—C2'—H2'2110.0H7C—O7—H7D108 (2)
C1'—C2'—H2'2110.0Ni1—O8—H8C120.5 (17)
H2'1—C2'—H2'2108.4Ni1—O8—H8D121.0 (18)
O2'—C3'—C499.6 (5)H8C—O8—H8D108 (2)
O2'—C3'—H3'1111.8Ni1—O9—H9C116.7 (16)
C4—C3'—H3'1111.8Ni1—O9—H9D116.4 (16)
O2'—C3'—H3'2111.8H9C—O9—H9D105.2 (18)
C4—C3'—H3'2111.8O10—Ni2—O10ii180.0
H3'1—C3'—H3'2109.6O10—Ni2—O6ii90.18 (6)
O1'—C10'—C9118.4 (5)O10ii—Ni2—O6ii89.82 (6)
O1'—C10'—H10C107.7O10—Ni2—O689.82 (6)
C9—C10'—H10C107.7O10ii—Ni2—O690.18 (6)
O1'—C10'—H10D107.7O6ii—Ni2—O6180.0
C9—C10'—H10D107.7O10—Ni2—O1190.39 (7)
H10C—C10'—H10D107.1O10ii—Ni2—O1189.61 (7)
C1'—O1'—C10'113.8 (5)O6ii—Ni2—O1192.17 (6)
C3'—O2'—C2'111.6 (6)O6—Ni2—O1187.83 (6)
O3—C4—C3'112.1 (6)O10—Ni2—O11ii89.61 (7)
O3—C4—C3109.0 (4)O10ii—Ni2—O11ii90.39 (7)
O3—C4—H4A109.9O6ii—Ni2—O11ii87.83 (6)
C3'—C4—H4A94.1O6—Ni2—O11ii92.17 (6)
C3—C4—H4A109.9O11—Ni2—O11ii180.0
O3—C4—H4B109.9Ni2—O6—H6C121.1 (15)
C3'—C4—H4B121.1Ni2—O6—H6D121.6 (16)
C3—C4—H4B109.9H6C—O6—H6D107.4 (19)
H4A—C4—H4B108.3Ni2—O10—H10E120.1 (17)
O3—C5—C6108.15 (17)Ni2—O10—H10F126.1 (17)
O3—C5—H5A110.1H10E—O10—H10F110 (2)
C6—C5—H5A110.1C11—O11—Ni2126.47 (12)
O3—C5—H5B110.1C11—O11—H11D114.5 (19)
C6—C5—H5B110.1Ni2—O11—H11D106.2 (19)
H5A—C5—H5B108.4O11—C11—H11A109.5
O4—C6—C5107.42 (18)O11—C11—H11B109.5
O4—C6—H6A110.2H11A—C11—H11B109.5
C5—C6—H6A110.2O11—C11—H11C109.5
O4—C6—H6B110.2H11A—C11—H11C109.5
C5—C6—H6B110.2H11B—C11—H11C109.5
H6A—C6—H6B108.5O13—N1—O12119.38 (18)
O4—C7—C8107.55 (17)O13—N1—O14120.18 (17)
O4—C7—H7A110.2O12—N1—O14120.43 (18)
C8—C7—H7A110.2O17—N2—O16119.98 (19)
O4—C7—H7B110.2O17—N2—O15120.66 (18)
C8—C7—H7B110.2O16—N2—O15119.36 (19)
H7A—C7—H7B108.5
O1—C1—C2—O264.6 (8)O1—C10—C9—O561.4 (4)
C9—C10—O1—C1173.3 (4)O1—C10—C9—C10'144.3 (15)
C2—C1—O1—C10159.6 (6)O1'—C10'—C9—O559.4 (6)
C1—C2—O2—C3166.3 (6)O1'—C10'—C9—C1045.3 (9)
C4—C3—O2—C282.2 (9)C6—C5—O3—C4162.14 (19)
O1'—C1'—C2'—O2'68.9 (11)C3'—C4—O3—C5162.4 (4)
C2'—C1'—O1'—C10'164.2 (7)C3—C4—O3—C5179.7 (3)
C9—C10'—O1'—C1'72.4 (8)C5—C6—O4—C7163.26 (17)
C4—C3'—O2'—C2'169.0 (7)C8—C7—O4—C6167.32 (17)
C1'—C2'—O2'—C3'160.9 (10)C10—C9—O5—C8163.6 (3)
O2'—C3'—C4—O365.9 (9)C10'—C9—O5—C8172.5 (3)
O2'—C3'—C4—C3148 (4)C7—C8—O5—C9165.81 (17)
O2—C3—C4—O360.8 (7)O10—Ni2—O11—C1199.27 (17)
O2—C3—C4—C3'43 (3)O10ii—Ni2—O11—C1180.73 (17)
O3—C5—C6—O469.2 (2)O6ii—Ni2—O11—C119.08 (17)
O4—C7—C8—O567.6 (2)O6—Ni2—O11—C11170.92 (17)
Symmetry codes: (i) x+1, y, z; (ii) x, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7C···O4i0.84 (2)1.94 (2)2.768 (2)170 (2)
O7—H7D···O2i0.79 (2)2.08 (2)2.765 (4)146 (3)
O7—H7D···O1i0.79 (2)2.11 (2)2.806 (3)147 (3)
O8—H8C···O17i0.83 (2)1.96 (2)2.773 (2)168 (2)
O8—H8D···O14i0.81 (2)1.95 (2)2.753 (2)176 (3)
O9—H9C···O12i0.84 (2)1.89 (2)2.727 (2)175 (2)
O9—H9D···O150.85 (2)1.88 (2)2.722 (2)172 (2)
O6—H6C···O30.84 (2)1.93 (2)2.771 (2)175 (2)
O6—H6D···O50.82 (2)2.06 (2)2.857 (2)165 (2)
O10—H10E···O16iii0.84 (2)1.88 (2)2.717 (2)173 (2)
O10—H10F···O13iv0.82 (2)1.91 (2)2.714 (2)169 (3)
O11—H11D···O20.77 (2)1.92 (2)2.692 (3)172 (3)
O11—H11D···O10.77 (2)2.35 (2)2.650 (4)104 (2)
Symmetry codes: (i) x+1, y, z; (iii) x+1, y, z+1; (iv) x+1/2, y1/2, z+1/2.
(4) top
Crystal data top
C10H20O5·H8N2NiO10·C10H20O5·H8N2NiO10F(000) = 4000
Mr = 950.11Dx = 1.644 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 9379 reflections
a = 15.352 (1) Åθ = 1.0–27.5°
b = 16.278 (1) ŵ = 1.09 mm1
c = 30.716 (2) ÅT = 90 K
V = 7675.9 (8) Å3Plate, pale green
Z = 80.50 × 0.40 × 0.05 mm
Data collection top
Nonius KappaCCD
diffractometer
8782 independent reflections
Radiation source: fine-focus sealed tube6081 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.044
Detector resolution: 18 pixels mm-1θmax = 27.5°, θmin = 1.3°
ω scans at fixed χ = 55°h = 1919
Absorption correction: multi-scan
Scalepack (Otwinowski & Minor, 2006)
k = 2121
Tmin = 0.612, Tmax = 0.948l = 3939
16396 measured reflections
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)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.079H atoms treated by a mixture of independent and constrained refinement
S = 1.02 w = 1/[σ2(Fo2) + (0.0319P)2 + 1.905P]
where P = (Fo2 + 2Fc2)/3
8782 reflections(Δ/σ)max = 0.001
553 parametersΔρmax = 0.33 e Å3
24 restraintsΔρmin = 0.49 e Å3
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C1_10.14539 (15)0.16617 (14)0.06705 (7)0.0195 (6)
H1A_10.08170.17540.06650.023*
H1B_10.16220.14930.09690.023*
C2_10.16971 (15)0.10065 (15)0.03516 (8)0.0203 (6)
H2A_10.13390.05090.04010.024*
H2B_10.15940.12010.00510.024*
C3_10.29823 (14)0.04043 (14)0.00473 (7)0.0151 (5)
H3A_10.27980.06710.02270.018*
H3B_10.27900.01760.00410.018*
C4_10.39568 (15)0.04472 (13)0.00931 (7)0.0145 (5)
H4A_10.41400.01960.03720.017*
H4B_10.42410.01450.01480.017*
C5_10.50952 (14)0.14529 (13)0.01824 (7)0.0144 (5)
H5A_10.54740.12620.00580.017*
H5B_10.52650.11590.04520.017*
C6_10.51933 (15)0.23604 (14)0.02440 (7)0.0147 (5)
H6A_10.58140.25000.02920.018*
H6B_10.49890.26540.00190.018*
C7_10.45482 (16)0.34689 (13)0.06255 (8)0.0187 (5)
H7A_10.42210.36450.03640.022*
H7B_10.51140.37600.06290.022*
C8_10.40388 (15)0.36749 (14)0.10302 (8)0.0187 (5)
H8A_10.43910.35320.12900.022*
H8B_10.39260.42740.10380.022*
C9_10.25254 (15)0.36402 (14)0.08258 (7)0.0190 (5)
H9A_10.26900.37520.05200.023*
H9B_10.23830.41690.09690.023*
C10_10.17564 (15)0.30740 (15)0.08417 (7)0.0199 (6)
H10A_10.16740.28680.11420.024*
H10B_10.12230.33740.07550.024*
O1_10.19023 (10)0.23990 (10)0.05517 (5)0.0193 (4)
O2_10.26007 (9)0.08184 (9)0.04116 (5)0.0160 (4)
O4_10.46875 (10)0.26024 (9)0.06134 (5)0.0141 (3)
O3_10.42025 (9)0.12940 (9)0.00819 (5)0.0134 (3)
O5_10.32250 (10)0.32442 (9)0.10487 (5)0.0160 (4)
Ni1_10.387899 (18)0.120446 (17)0.168692 (8)0.01125 (8)
O6_10.39832 (10)0.11150 (10)0.23501 (5)0.0134 (3)
H6C_10.3598 (12)0.0916 (13)0.2494 (7)0.020*
H6D_10.4228 (13)0.1474 (12)0.2486 (7)0.020*
O7_10.38128 (10)0.13049 (10)0.10288 (5)0.0143 (4)
H7C_10.3369 (12)0.1189 (14)0.0897 (7)0.021*
H7D_10.4020 (14)0.1724 (11)0.0918 (7)0.021*
O9_10.46923 (11)0.02073 (9)0.16578 (5)0.0157 (4)
H9C_10.4894 (14)0.0105 (14)0.1421 (6)0.024*
H9D_10.4347 (13)0.0179 (12)0.1713 (7)0.024*
O11_10.30554 (10)0.21920 (9)0.17369 (5)0.0137 (3)
H11C_10.3071 (15)0.2517 (13)0.1529 (5)0.021*
H11D_10.3203 (15)0.2485 (13)0.1951 (5)0.021*
N1_10.55316 (12)0.21331 (12)0.14650 (6)0.0148 (4)
O10_10.48648 (9)0.20875 (9)0.17088 (5)0.0139 (3)
O12_10.57758 (10)0.15271 (9)0.12493 (5)0.0157 (4)
O13_10.59262 (10)0.28071 (9)0.14543 (5)0.0181 (4)
N2_10.26347 (13)0.02339 (11)0.18283 (6)0.0167 (4)
O8_10.27490 (10)0.05012 (9)0.16881 (5)0.0164 (4)
O14_10.32834 (11)0.06858 (10)0.18961 (6)0.0265 (4)
O15_10.18864 (10)0.04778 (10)0.18921 (5)0.0232 (4)
C1_20.16985 (15)0.13064 (14)0.26939 (7)0.0168 (5)
H1A_20.18660.12030.23880.020*
H1B_20.10690.14360.27030.020*
C2_20.18859 (14)0.05635 (14)0.29668 (7)0.0168 (5)
H2A_20.17650.06850.32770.020*
H2B_20.15070.01020.28750.020*
C3_20.31373 (15)0.01046 (14)0.32739 (7)0.0164 (5)
H3A_20.29480.06850.32600.020*
H3B_20.29250.01340.35510.020*
C4_20.41098 (15)0.00585 (13)0.32567 (7)0.0178 (5)
H4A_20.43680.04150.34840.021*
H4B_20.43220.02460.29690.021*
C5_20.52594 (14)0.09339 (14)0.32642 (7)0.0162 (5)
H5A_20.54520.07050.29810.019*
H5B_20.56050.06730.34990.019*
C6_20.53881 (15)0.18459 (14)0.32709 (7)0.0150 (5)
H6A_20.51400.20790.35420.018*
H6B_20.60180.19760.32630.018*
C7_20.48296 (15)0.30636 (14)0.29414 (7)0.0171 (5)
H7A_20.53950.33500.29710.021*
H7B_20.44740.31830.32030.021*
C8_20.43624 (14)0.33491 (13)0.25355 (7)0.0166 (5)
H8A_20.42580.39480.25550.020*
H8B_20.47370.32470.22790.020*
C9_20.28370 (14)0.32793 (14)0.27203 (7)0.0160 (5)
H9A_20.27160.38450.26190.019*
H9B_20.29860.33010.30340.019*
C10_20.20495 (14)0.27471 (13)0.26520 (7)0.0162 (5)
H10A_20.15260.30190.27730.019*
H10B_20.19540.26550.23370.019*
O1_20.21936 (10)0.19793 (9)0.28671 (5)0.0170 (4)
O2_20.27822 (10)0.03428 (9)0.29129 (5)0.0148 (3)
O3_20.43523 (9)0.07774 (9)0.33284 (5)0.0143 (3)
O4_20.49642 (10)0.21979 (9)0.28999 (5)0.0147 (4)
O5_20.35481 (10)0.29357 (9)0.24779 (5)0.0152 (3)
Ni2_20.310559 (18)0.224144 (17)0.424075 (9)0.01100 (8)
O6_20.31286 (10)0.24637 (10)0.48896 (5)0.0142 (3)
H6C_20.2689 (11)0.2481 (14)0.5040 (7)0.021*
H6D_20.3441 (13)0.2865 (12)0.4962 (7)0.021*
O7_20.31825 (11)0.19572 (10)0.35948 (5)0.0165 (4)
H7C_20.2802 (12)0.1986 (14)0.3402 (7)0.025*
H7D_20.3539 (13)0.1613 (13)0.3528 (7)0.025*
O8_20.21410 (10)0.13883 (10)0.43534 (5)0.0157 (4)
H8C_20.2414 (14)0.0947 (11)0.4327 (7)0.024*
H8D_20.1763 (13)0.1397 (14)0.4160 (7)0.024*
O11_20.21665 (11)0.31105 (10)0.41521 (5)0.0162 (4)
H11C_20.1788 (13)0.3011 (13)0.3963 (7)0.024*
H11D_20.2432 (14)0.3516 (12)0.4071 (7)0.024*
N1_20.41446 (13)0.38312 (12)0.40661 (6)0.0149 (4)
O10_20.41505 (10)0.30683 (9)0.41585 (5)0.0140 (3)
O12_20.48439 (10)0.42195 (9)0.40797 (5)0.0181 (4)
O13_20.34503 (11)0.41863 (10)0.39621 (6)0.0262 (4)
N2_20.41339 (13)0.06660 (12)0.43212 (6)0.0166 (4)
O9_20.41386 (9)0.14503 (9)0.43280 (5)0.0140 (3)
O14_20.48365 (10)0.02978 (10)0.43117 (6)0.0246 (4)
O15_20.34260 (10)0.02762 (9)0.43221 (5)0.0193 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C1_10.0139 (13)0.0239 (14)0.0206 (13)0.0033 (11)0.0032 (10)0.0028 (11)
C2_10.0130 (13)0.0264 (15)0.0214 (13)0.0017 (11)0.0012 (10)0.0009 (11)
C3_10.0188 (13)0.0140 (12)0.0126 (11)0.0025 (10)0.0022 (10)0.0008 (9)
C4_10.0205 (13)0.0104 (12)0.0126 (11)0.0006 (10)0.0007 (10)0.0004 (9)
C5_10.0131 (13)0.0174 (13)0.0127 (12)0.0024 (10)0.0007 (10)0.0004 (9)
C6_10.0129 (12)0.0178 (13)0.0134 (12)0.0020 (10)0.0021 (10)0.0009 (10)
C7_10.0214 (14)0.0117 (13)0.0230 (13)0.0025 (10)0.0021 (11)0.0005 (10)
C8_10.0216 (14)0.0125 (13)0.0220 (13)0.0025 (10)0.0004 (11)0.0030 (10)
C9_10.0257 (14)0.0181 (13)0.0132 (12)0.0074 (11)0.0026 (11)0.0005 (10)
C10_10.0193 (14)0.0242 (14)0.0162 (12)0.0086 (11)0.0012 (10)0.0026 (10)
O1_10.0201 (9)0.0222 (9)0.0156 (8)0.0033 (7)0.0056 (7)0.0024 (7)
O2_10.0108 (8)0.0246 (9)0.0125 (8)0.0001 (7)0.0006 (7)0.0030 (7)
O4_10.0185 (9)0.0109 (8)0.0129 (8)0.0010 (7)0.0031 (7)0.0013 (6)
O3_10.0102 (8)0.0136 (8)0.0163 (8)0.0002 (7)0.0012 (7)0.0021 (6)
O5_10.0170 (9)0.0138 (9)0.0172 (8)0.0001 (7)0.0023 (7)0.0022 (7)
Ni1_10.01291 (16)0.01245 (15)0.00839 (14)0.00064 (12)0.00054 (12)0.00014 (12)
O6_10.0168 (9)0.0153 (9)0.0081 (8)0.0040 (7)0.0011 (7)0.0000 (6)
O7_10.0178 (9)0.0168 (9)0.0084 (8)0.0053 (7)0.0013 (7)0.0014 (7)
O9_10.0182 (9)0.0152 (9)0.0138 (9)0.0021 (7)0.0050 (7)0.0002 (7)
O11_10.0170 (9)0.0139 (9)0.0103 (8)0.0019 (7)0.0005 (7)0.0003 (6)
N1_10.0119 (10)0.0220 (12)0.0103 (10)0.0002 (9)0.0027 (8)0.0019 (8)
O10_10.0107 (8)0.0178 (9)0.0133 (8)0.0034 (7)0.0062 (7)0.0007 (7)
O12_10.0161 (9)0.0177 (9)0.0134 (8)0.0036 (7)0.0030 (7)0.0018 (7)
O13_10.0177 (9)0.0172 (9)0.0194 (9)0.0076 (7)0.0012 (7)0.0004 (7)
N2_10.0217 (12)0.0159 (11)0.0126 (10)0.0006 (9)0.0015 (9)0.0012 (8)
O8_10.0176 (9)0.0121 (8)0.0196 (9)0.0027 (7)0.0020 (7)0.0041 (7)
O14_10.0206 (10)0.0170 (9)0.0420 (11)0.0051 (8)0.0040 (8)0.0093 (8)
O15_10.0161 (9)0.0251 (10)0.0284 (10)0.0069 (8)0.0001 (8)0.0062 (8)
C1_20.0116 (12)0.0211 (14)0.0178 (12)0.0016 (10)0.0013 (10)0.0056 (10)
C2_20.0118 (12)0.0176 (13)0.0210 (13)0.0023 (10)0.0030 (10)0.0059 (10)
C3_20.0229 (14)0.0128 (12)0.0137 (12)0.0040 (10)0.0017 (11)0.0009 (9)
C4_20.0243 (14)0.0122 (12)0.0169 (12)0.0007 (10)0.0036 (11)0.0013 (10)
C5_20.0133 (12)0.0218 (13)0.0135 (12)0.0013 (10)0.0004 (10)0.0019 (10)
C6_20.0113 (12)0.0221 (13)0.0116 (11)0.0013 (10)0.0016 (10)0.0024 (10)
C7_20.0173 (13)0.0137 (13)0.0204 (13)0.0009 (10)0.0017 (10)0.0052 (10)
C8_20.0196 (13)0.0128 (12)0.0173 (12)0.0014 (10)0.0033 (10)0.0017 (10)
C9_20.0191 (13)0.0162 (13)0.0128 (12)0.0048 (10)0.0011 (10)0.0008 (10)
C10_20.0182 (13)0.0171 (13)0.0133 (12)0.0071 (10)0.0003 (10)0.0014 (10)
O1_20.0225 (9)0.0140 (9)0.0144 (8)0.0016 (7)0.0073 (7)0.0012 (7)
O2_20.0137 (8)0.0179 (9)0.0128 (8)0.0022 (7)0.0004 (7)0.0015 (7)
O3_20.0132 (8)0.0131 (8)0.0167 (8)0.0028 (7)0.0003 (7)0.0021 (7)
O4_20.0176 (9)0.0150 (9)0.0115 (8)0.0000 (7)0.0035 (7)0.0007 (6)
O5_20.0154 (9)0.0158 (8)0.0143 (8)0.0024 (7)0.0000 (7)0.0027 (7)
Ni2_20.01126 (15)0.01253 (16)0.00920 (14)0.00050 (12)0.00029 (12)0.00065 (11)
O6_20.0128 (9)0.0185 (9)0.0112 (8)0.0048 (7)0.0015 (7)0.0031 (7)
O7_20.0169 (10)0.0220 (10)0.0106 (8)0.0055 (7)0.0033 (7)0.0050 (7)
O8_20.0129 (9)0.0163 (9)0.0178 (9)0.0001 (7)0.0026 (7)0.0011 (7)
O11_20.0157 (9)0.0149 (9)0.0180 (9)0.0005 (7)0.0048 (7)0.0003 (7)
N1_20.0186 (11)0.0166 (11)0.0096 (10)0.0023 (9)0.0010 (8)0.0003 (8)
O10_20.0155 (9)0.0105 (8)0.0160 (8)0.0026 (7)0.0009 (7)0.0001 (6)
O12_20.0146 (9)0.0182 (9)0.0216 (9)0.0080 (7)0.0000 (7)0.0030 (7)
O13_20.0164 (9)0.0213 (10)0.0409 (11)0.0005 (8)0.0068 (8)0.0117 (8)
N2_20.0196 (12)0.0139 (11)0.0163 (11)0.0020 (9)0.0024 (9)0.0014 (8)
O9_20.0134 (8)0.0109 (8)0.0177 (8)0.0032 (7)0.0011 (7)0.0010 (6)
O14_20.0155 (9)0.0154 (9)0.0427 (11)0.0066 (8)0.0024 (8)0.0030 (8)
O15_20.0155 (9)0.0148 (9)0.0278 (10)0.0041 (7)0.0013 (7)0.0038 (7)
Geometric parameters (Å, º) top
C1_1—O1_11.431 (3)C1_2—O1_21.435 (3)
C1_1—C2_11.496 (3)C1_2—C2_21.499 (3)
C1_1—H1A_10.9900C1_2—H1A_20.9900
C1_1—H1B_10.9900C1_2—H1B_20.9900
C2_1—O2_11.432 (3)C2_2—O2_21.432 (3)
C2_1—H2A_10.9900C2_2—H2A_20.9900
C2_1—H2B_10.9900C2_2—H2B_20.9900
C3_1—O2_11.432 (2)C3_2—O2_21.434 (2)
C3_1—C4_11.504 (3)C3_2—C4_21.496 (3)
C3_1—H3A_10.9900C3_2—H3A_20.9900
C3_1—H3B_10.9900C3_2—H3B_20.9900
C4_1—O3_11.429 (2)C4_2—O3_21.428 (2)
C4_1—H4A_10.9900C4_2—H4A_20.9900
C4_1—H4B_10.9900C4_2—H4B_20.9900
C5_1—O3_11.428 (3)C5_2—O3_21.429 (3)
C5_1—C6_11.497 (3)C5_2—C6_21.498 (3)
C5_1—H5A_10.9900C5_2—H5A_20.9900
C5_1—H5B_10.9900C5_2—H5B_20.9900
C6_1—O4_11.430 (2)C6_2—O4_21.432 (2)
C6_1—H6A_10.9900C6_2—H6A_20.9900
C6_1—H6B_10.9900C6_2—H6B_20.9900
C7_1—O4_11.427 (3)C7_2—O4_21.430 (3)
C7_1—C8_11.506 (3)C7_2—C8_21.512 (3)
C7_1—H7A_10.9900C7_2—H7A_20.9900
C7_1—H7B_10.9900C7_2—H7B_20.9900
C8_1—O5_11.434 (3)C8_2—O5_21.431 (3)
C8_1—H8A_10.9900C8_2—H8A_20.9900
C8_1—H8B_10.9900C8_2—H8B_20.9900
C9_1—O5_11.428 (3)C9_2—O5_21.435 (2)
C9_1—C10_11.498 (3)C9_2—C10_21.502 (3)
C9_1—H9A_10.9900C9_2—H9A_20.9900
C9_1—H9B_10.9900C9_2—H9B_20.9900
C10_1—O1_11.432 (3)C10_2—O1_21.431 (3)
C10_1—H10A_10.9900C10_2—H10A_20.9900
C10_1—H10B_10.9900C10_2—H10B_20.9900
Ni1_1—O7_12.0307 (15)Ni2_2—O6_22.0257 (15)
Ni1_1—O6_12.0486 (14)Ni2_2—O11_22.0381 (16)
Ni1_1—O9_12.0498 (16)Ni2_2—O7_22.0408 (15)
Ni1_1—O11_12.0509 (15)Ni2_2—O8_22.0594 (16)
Ni1_1—O8_12.0784 (15)Ni2_2—O9_22.0604 (15)
Ni1_1—O10_12.0883 (15)Ni2_2—O10_22.1092 (15)
O6_1—H6C_10.806 (15)O6_2—H6C_20.817 (15)
O6_1—H6D_10.810 (15)O6_2—H6D_20.840 (15)
O7_1—H7C_10.814 (15)O7_2—H7C_20.834 (15)
O7_1—H7D_10.826 (15)O7_2—H7D_20.810 (15)
O9_1—H9C_10.809 (15)O8_2—H8C_20.836 (15)
O9_1—H9D_10.840 (15)O8_2—H8D_20.831 (15)
O11_1—H11C_10.830 (15)O11_2—H11C_20.838 (15)
O11_1—H11D_10.844 (15)O11_2—H11D_20.815 (15)
N1_1—O12_11.246 (2)N1_2—O12_21.247 (2)
N1_1—O13_11.254 (2)N1_2—O13_21.254 (2)
N1_1—O10_11.270 (2)N1_2—O10_21.274 (2)
N2_1—O15_11.231 (2)N2_2—O14_21.234 (2)
N2_1—O14_11.255 (2)N2_2—O15_21.258 (2)
N2_1—O8_11.284 (2)N2_2—O9_21.277 (2)
O1_1—C1_1—C2_1108.12 (18)O1_2—C1_2—C2_2107.86 (18)
O1_1—C1_1—H1A_1110.1O1_2—C1_2—H1A_2110.1
C2_1—C1_1—H1A_1110.1C2_2—C1_2—H1A_2110.1
O1_1—C1_1—H1B_1110.1O1_2—C1_2—H1B_2110.1
C2_1—C1_1—H1B_1110.1C2_2—C1_2—H1B_2110.1
H1A_1—C1_1—H1B_1108.4H1A_2—C1_2—H1B_2108.4
O2_1—C2_1—C1_1108.06 (18)O2_2—C2_2—C1_2108.79 (18)
O2_1—C2_1—H2A_1110.1O2_2—C2_2—H2A_2109.9
C1_1—C2_1—H2A_1110.1C1_2—C2_2—H2A_2109.9
O2_1—C2_1—H2B_1110.1O2_2—C2_2—H2B_2109.9
C1_1—C2_1—H2B_1110.1C1_2—C2_2—H2B_2109.9
H2A_1—C2_1—H2B_1108.4H2A_2—C2_2—H2B_2108.3
O2_1—C3_1—C4_1108.18 (17)O2_2—C3_2—C4_2109.06 (18)
O2_1—C3_1—H3A_1110.1O2_2—C3_2—H3A_2109.9
C4_1—C3_1—H3A_1110.1C4_2—C3_2—H3A_2109.9
O2_1—C3_1—H3B_1110.1O2_2—C3_2—H3B_2109.9
C4_1—C3_1—H3B_1110.1C4_2—C3_2—H3B_2109.9
H3A_1—C3_1—H3B_1108.4H3A_2—C3_2—H3B_2108.3
O3_1—C4_1—C3_1107.76 (18)O3_2—C4_2—C3_2107.62 (18)
O3_1—C4_1—H4A_1110.2O3_2—C4_2—H4A_2110.2
C3_1—C4_1—H4A_1110.2C3_2—C4_2—H4A_2110.2
O3_1—C4_1—H4B_1110.2O3_2—C4_2—H4B_2110.2
C3_1—C4_1—H4B_1110.2C3_2—C4_2—H4B_2110.2
H4A_1—C4_1—H4B_1108.5H4A_2—C4_2—H4B_2108.5
O3_1—C5_1—C6_1107.62 (18)O3_2—C5_2—C6_2107.65 (18)
O3_1—C5_1—H5A_1110.2O3_2—C5_2—H5A_2110.2
C6_1—C5_1—H5A_1110.2C6_2—C5_2—H5A_2110.2
O3_1—C5_1—H5B_1110.2O3_2—C5_2—H5B_2110.2
C6_1—C5_1—H5B_1110.2C6_2—C5_2—H5B_2110.2
H5A_1—C5_1—H5B_1108.5H5A_2—C5_2—H5B_2108.5
O4_1—C6_1—C5_1108.51 (17)O4_2—C6_2—C5_2109.01 (17)
O4_1—C6_1—H6A_1110.0O4_2—C6_2—H6A_2109.9
C5_1—C6_1—H6A_1110.0C5_2—C6_2—H6A_2109.9
O4_1—C6_1—H6B_1110.0O4_2—C6_2—H6B_2109.9
C5_1—C6_1—H6B_1110.0C5_2—C6_2—H6B_2109.9
H6A_1—C6_1—H6B_1108.4H6A_2—C6_2—H6B_2108.3
O4_1—C7_1—C8_1108.62 (18)O4_2—C7_2—C8_2107.33 (17)
O4_1—C7_1—H7A_1110.0O4_2—C7_2—H7A_2110.2
C8_1—C7_1—H7A_1110.0C8_2—C7_2—H7A_2110.2
O4_1—C7_1—H7B_1110.0O4_2—C7_2—H7B_2110.2
C8_1—C7_1—H7B_1110.0C8_2—C7_2—H7B_2110.2
H7A_1—C7_1—H7B_1108.3H7A_2—C7_2—H7B_2108.5
O5_1—C8_1—C7_1112.11 (18)O5_2—C8_2—C7_2111.84 (18)
O5_1—C8_1—H8A_1109.2O5_2—C8_2—H8A_2109.2
C7_1—C8_1—H8A_1109.2C7_2—C8_2—H8A_2109.2
O5_1—C8_1—H8B_1109.2O5_2—C8_2—H8B_2109.2
C7_1—C8_1—H8B_1109.2C7_2—C8_2—H8B_2109.2
H8A_1—C8_1—H8B_1107.9H8A_2—C8_2—H8B_2107.9
O5_1—C9_1—C10_1107.42 (18)O5_2—C9_2—C10_2108.36 (17)
O5_1—C9_1—H9A_1110.2O5_2—C9_2—H9A_2110.0
C10_1—C9_1—H9A_1110.2C10_2—C9_2—H9A_2110.0
O5_1—C9_1—H9B_1110.2O5_2—C9_2—H9B_2110.0
C10_1—C9_1—H9B_1110.2C10_2—C9_2—H9B_2110.0
H9A_1—C9_1—H9B_1108.5H9A_2—C9_2—H9B_2108.4
O1_1—C10_1—C9_1109.17 (18)O1_2—C10_2—C9_2108.35 (17)
O1_1—C10_1—H10A_1109.8O1_2—C10_2—H10A_2110.0
C9_1—C10_1—H10A_1109.8C9_2—C10_2—H10A_2110.0
O1_1—C10_1—H10B_1109.8O1_2—C10_2—H10B_2110.0
C9_1—C10_1—H10B_1109.8C9_2—C10_2—H10B_2110.0
H10A_1—C10_1—H10B_1108.3H10A_2—C10_2—H10B_2108.4
C1_1—O1_1—C10_1114.19 (17)C10_2—O1_2—C1_2114.42 (16)
C3_1—O2_1—C2_1113.35 (16)C2_2—O2_2—C3_2113.79 (16)
C7_1—O4_1—C6_1111.98 (16)C4_2—O3_2—C5_2113.74 (17)
C5_1—O3_1—C4_1115.00 (16)C7_2—O4_2—C6_2112.89 (16)
C9_1—O5_1—C8_1114.57 (17)C8_2—O5_2—C9_2114.65 (16)
O7_1—Ni1_1—O6_1178.31 (7)O6_2—Ni2_2—O11_291.14 (6)
O7_1—Ni1_1—O9_192.91 (6)O6_2—Ni2_2—O7_2174.84 (7)
O6_1—Ni1_1—O9_186.54 (6)O11_2—Ni2_2—O7_293.92 (6)
O7_1—Ni1_1—O11_188.89 (6)O6_2—Ni2_2—O8_288.14 (6)
O6_1—Ni1_1—O11_191.68 (6)O11_2—Ni2_2—O8_288.96 (7)
O9_1—Ni1_1—O11_1178.10 (6)O7_2—Ni2_2—O8_292.99 (6)
O7_1—Ni1_1—O8_190.25 (6)O6_2—Ni2_2—O9_288.29 (6)
O6_1—Ni1_1—O8_191.39 (6)O11_2—Ni2_2—O9_2174.67 (6)
O9_1—Ni1_1—O8_194.14 (6)O7_2—Ni2_2—O9_286.58 (6)
O11_1—Ni1_1—O8_185.24 (6)O8_2—Ni2_2—O9_296.32 (6)
O7_1—Ni1_1—O10_190.74 (6)O6_2—Ni2_2—O10_289.46 (6)
O6_1—Ni1_1—O10_187.72 (6)O11_2—Ni2_2—O10_294.54 (6)
O9_1—Ni1_1—O10_196.03 (6)O7_2—Ni2_2—O10_289.09 (6)
O11_1—Ni1_1—O10_184.54 (6)O8_2—Ni2_2—O10_2175.80 (6)
O8_1—Ni1_1—O10_1169.72 (6)O9_2—Ni2_2—O10_280.16 (6)
Ni1_1—O6_1—H6C_1121.0 (16)Ni2_2—O6_2—H6C_2123.1 (16)
Ni1_1—O6_1—H6D_1119.8 (16)Ni2_2—O6_2—H6D_2114.2 (16)
H6C_1—O6_1—H6D_1110 (2)H6C_2—O6_2—H6D_2107.2 (19)
Ni1_1—O7_1—H7C_1121.2 (16)Ni2_2—O7_2—H7C_2129.7 (16)
Ni1_1—O7_1—H7D_1117.2 (16)Ni2_2—O7_2—H7D_2116.3 (16)
H7C_1—O7_1—H7D_1108.0 (19)H7C_2—O7_2—H7D_2109.4 (19)
Ni1_1—O9_1—H9C_1115.8 (17)Ni2_2—O8_2—H8C_2101.7 (17)
Ni1_1—O9_1—H9D_1101.5 (16)Ni2_2—O8_2—H8D_2111.7 (17)
H9C_1—O9_1—H9D_1105.7 (19)H8C_2—O8_2—H8D_2107.1 (19)
Ni1_1—O11_1—H11C_1115.1 (16)Ni2_2—O11_2—H11C_2116.7 (16)
Ni1_1—O11_1—H11D_1109.6 (16)Ni2_2—O11_2—H11D_2104.5 (18)
H11C_1—O11_1—H11D_1103.5 (18)H11C_2—O11_2—H11D_2106.9 (19)
O12_1—N1_1—O13_1122.23 (18)O12_2—N1_2—O13_2120.47 (18)
O12_1—N1_1—O10_1120.63 (18)O12_2—N1_2—O10_2118.72 (18)
O13_1—N1_1—O10_1117.14 (18)O13_2—N1_2—O10_2120.81 (18)
N1_1—O10_1—Ni1_1127.24 (13)N1_2—O10_2—Ni2_2130.04 (14)
O15_1—N2_1—O14_1121.65 (19)O14_2—N2_2—O15_2120.66 (18)
O15_1—N2_1—O8_1118.79 (19)O14_2—N2_2—O9_2118.75 (19)
O14_1—N2_1—O8_1119.56 (19)O15_2—N2_2—O9_2120.60 (18)
N2_1—O8_1—Ni1_1128.91 (14)N2_2—O9_2—Ni2_2128.20 (13)
O1_1—C1_1—C2_1—O2_167.2 (2)O10_1—Ni1_1—O8_1—N2_1143.6 (3)
O2_1—C3_1—C4_1—O3_162.2 (2)O1_2—C1_2—C2_2—O2_265.5 (2)
O3_1—C5_1—C6_1—O4_164.0 (2)O2_2—C3_2—C4_2—O3_266.1 (2)
O4_1—C7_1—C8_1—O5_157.5 (2)O3_2—C5_2—C6_2—O4_266.4 (2)
O5_1—C9_1—C10_1—O1_173.0 (2)O4_2—C7_2—C8_2—O5_258.8 (2)
C2_1—C1_1—O1_1—C10_1177.60 (18)O5_2—C9_2—C10_2—O1_269.4 (2)
C9_1—C10_1—O1_1—C1_1153.14 (18)C9_2—C10_2—O1_2—C1_2155.74 (17)
C4_1—C3_1—O2_1—C2_1164.74 (18)C2_2—C1_2—O1_2—C10_2177.10 (17)
C1_1—C2_1—O2_1—C3_1161.34 (18)C1_2—C2_2—O2_2—C3_2154.95 (18)
C8_1—C7_1—O4_1—C6_1178.13 (18)C4_2—C3_2—O2_2—C2_2161.26 (18)
C5_1—C6_1—O4_1—C7_1163.88 (18)C3_2—C4_2—O3_2—C5_2172.22 (17)
C6_1—C5_1—O3_1—C4_1168.75 (17)C6_2—C5_2—O3_2—C4_2170.00 (17)
C3_1—C4_1—O3_1—C5_1171.62 (16)C8_2—C7_2—O4_2—C6_2178.73 (17)
C10_1—C9_1—O5_1—C8_1174.72 (17)C5_2—C6_2—O4_2—C7_2162.84 (18)
C7_1—C8_1—O5_1—C9_185.8 (2)C7_2—C8_2—O5_2—C9_283.0 (2)
O12_1—N1_1—O10_1—Ni1_117.8 (3)C10_2—C9_2—O5_2—C8_2175.97 (17)
O13_1—N1_1—O10_1—Ni1_1162.49 (13)O12_2—N1_2—O10_2—Ni2_2172.34 (13)
O7_1—Ni1_1—O10_1—N1_145.39 (16)O13_2—N1_2—O10_2—Ni2_27.9 (3)
O6_1—Ni1_1—O10_1—N1_1133.88 (16)O6_2—Ni2_2—O10_2—N1_293.83 (16)
O9_1—Ni1_1—O10_1—N1_147.61 (16)O11_2—Ni2_2—O10_2—N1_22.74 (16)
O11_1—Ni1_1—O10_1—N1_1134.21 (16)O7_2—Ni2_2—O10_2—N1_291.13 (16)
O8_1—Ni1_1—O10_1—N1_1140.9 (3)O9_2—Ni2_2—O10_2—N1_2177.81 (16)
O15_1—N2_1—O8_1—Ni1_1163.60 (14)O14_2—N2_2—O9_2—Ni2_2168.68 (14)
O14_1—N2_1—O8_1—Ni1_116.5 (3)O15_2—N2_2—O9_2—Ni2_211.0 (3)
O7_1—Ni1_1—O8_1—N2_1120.88 (17)O6_2—Ni2_2—O9_2—N2_2105.75 (16)
O6_1—Ni1_1—O8_1—N2_158.68 (17)O7_2—Ni2_2—O9_2—N2_274.82 (16)
O9_1—Ni1_1—O8_1—N2_127.94 (17)O8_2—Ni2_2—O9_2—N2_217.81 (16)
O11_1—Ni1_1—O8_1—N2_1150.26 (17)O10_2—Ni2_2—O9_2—N2_2164.50 (16)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6_1—H6C_1···O2_20.81 (2)2.02 (2)2.823 (2)171 (2)
O6_1—H6D_1···O4_20.81 (2)2.07 (2)2.868 (2)169 (2)
O7_1—H7C_1···O2_10.81 (2)2.00 (2)2.772 (2)159 (2)
O7_1—H7D_1···O4_10.83 (2)1.99 (2)2.809 (2)170 (2)
O9_1—H9C_1···O12_2i0.81 (2)2.15 (2)2.868 (2)149 (2)
O9_1—H9D_1···O14_10.84 (2)1.91 (2)2.707 (2)157 (2)
O11_1—H11C_1···O5_10.83 (2)1.91 (2)2.733 (2)174 (2)
O11_1—H11D_1···O5_20.84 (2)1.85 (2)2.687 (2)169 (2)
O6_2—H6C_2···O1_1ii0.82 (2)1.99 (2)2.780 (2)161 (2)
O6_2—H6D_2···O3_1ii0.84 (2)1.84 (2)2.675 (2)174 (2)
O7_2—H7C_2···O1_20.83 (2)1.89 (2)2.702 (2)165 (2)
O7_2—H7D_2···O3_20.81 (2)1.95 (2)2.754 (2)176 (2)
O8_2—H8C_2···O15_20.84 (2)1.90 (2)2.679 (2)155 (2)
O8_2—H8D_2···O12_1iii0.83 (2)1.98 (2)2.805 (2)172 (2)
O11_2—H11C_2···O13_1iii0.84 (2)1.87 (2)2.709 (2)179 (3)
O11_2—H11D_2···O13_20.82 (2)1.94 (2)2.700 (2)156 (2)
Symmetry codes: (i) x+1, y1/2, z+1/2; (ii) x, y+1/2, z+1/2; (iii) x1/2, y, z+1/2.
(5) top
Crystal data top
C10H20O5·C2H7N3NiO8·C2H3NZ = 4
Mr = 521.13F(000) = 1096
Triclinic, P1Dx = 1.519 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 12.144 (1) ÅCell parameters from 9946 reflections
b = 12.137 (1) Åθ = 1.0–27.5°
c = 16.039 (1) ŵ = 0.92 mm1
α = 90.12 (1)°T = 90 K
β = 105.47 (1)°Parallelepiped, pale green
γ = 90.04 (1)°0.20 × 0.10 × 0.08 mm
V = 2278.4 (3) Å3
Data collection top
Nonius KappaCCD
diffractometer
10381 independent reflections
Radiation source: fine-focus sealed tube7375 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.051
Detector resolution: 18 pixels mm-1θmax = 27.5°, θmin = 1.3°
ω scans at fixed χ = 55°h = 1515
Absorption correction: multi-scan
Scalepack (Otwinowski & Minor, 2006)
k = 1515
Tmin = 0.837, Tmax = 0.930l = 2020
19489 measured reflections
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)] = 0.043Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.095H atoms treated by a mixture of independent and constrained refinement
S = 1.00 w = 1/[σ2(Fo2) + (0.0395P)2]
where P = (Fo2 + 2Fc2)/3
10381 reflections(Δ/σ)max = 0.001
606 parametersΔρmax = 0.77 e Å3
12 restraintsΔρmin = 0.57 e Å3
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C1_10.0603 (3)0.1550 (3)0.3048 (3)0.0239 (10)
H1A_10.06220.16880.24430.029*
H1B_10.01960.13940.30510.029*
C2_10.1352 (3)0.0590 (4)0.3411 (3)0.0242 (11)
H2A_10.13430.04560.40170.029*
H2B_10.10780.00830.30680.029*
C3_10.3322 (3)0.0048 (3)0.3745 (3)0.0250 (10)
H3A_10.32220.06110.33680.030*
H3B_10.32310.01770.43160.030*
C4_10.4484 (3)0.0530 (3)0.3849 (3)0.0211 (10)
H4A_10.50680.00590.39890.025*
H4B_10.45260.08850.33030.025*
C5_10.5705 (3)0.1978 (3)0.4632 (2)0.0194 (9)
H5A_10.62820.15370.44430.023*
H5B_10.60260.21630.52510.023*
C6_10.5479 (3)0.3024 (3)0.4115 (2)0.0198 (9)
H6A_10.61910.34590.42040.024*
H6B_10.51880.28530.34910.024*
C7_10.4349 (3)0.4646 (3)0.3965 (3)0.0214 (10)
H7A_10.42830.45550.33400.026*
H7B_10.49400.52110.42010.026*
C8_10.3226 (3)0.4990 (3)0.4101 (2)0.0219 (10)
H8A_10.32110.48370.47040.026*
H8B_10.31080.57900.39940.026*
C9_10.1248 (3)0.4424 (4)0.3682 (3)0.0225 (11)
H9A_10.08770.51410.34940.027*
H9B_10.13300.43390.43100.027*
C10_10.0546 (3)0.3509 (3)0.3192 (3)0.0218 (10)
H10A_10.02560.35770.32200.026*
H10B_10.05580.35310.25780.026*
O1_10.10252 (19)0.2501 (2)0.35782 (15)0.0199 (6)
O2_10.2488 (2)0.0858 (2)0.33695 (17)0.0187 (6)
O3_10.4696 (2)0.1332 (2)0.45365 (16)0.0198 (6)
O4_10.4652 (2)0.3627 (2)0.44052 (17)0.0203 (7)
O5_10.2342 (2)0.4378 (2)0.35084 (17)0.0217 (7)
Ni1_10.30366 (4)0.26565 (4)0.13580 (3)0.01610 (12)
O6_10.3049 (2)0.2687 (2)0.26255 (16)0.0164 (6)
H6C_10.291 (3)0.2058 (15)0.277 (2)0.025*
H6D_10.270 (3)0.311 (2)0.289 (2)0.025*
O7_10.29221 (19)0.2614 (3)0.00815 (15)0.0261 (7)
H7C_10.3478 (18)0.271 (3)0.011 (2)0.039*
H7D_10.2352 (18)0.252 (4)0.0330 (17)0.039*
N1_10.2200 (3)0.0417 (3)0.1387 (2)0.0255 (9)
O8_10.3104 (2)0.0977 (2)0.14659 (16)0.0248 (6)
O9_10.1251 (2)0.0865 (2)0.11432 (16)0.0348 (7)
O10_10.2264 (2)0.0576 (2)0.15822 (17)0.0331 (7)
N2_10.1861 (3)0.4366 (3)0.1186 (2)0.0274 (9)
O11_10.2950 (2)0.4387 (2)0.13714 (19)0.0219 (6)
O12_10.1393 (2)0.3419 (2)0.10731 (18)0.0253 (7)
O13_10.1297 (3)0.5217 (3)0.1125 (2)0.0448 (9)
C11_10.6921 (3)0.2426 (4)0.2551 (2)0.0259 (9)
H11A_10.71240.30730.29280.039*
H11B_10.74080.23970.21530.039*
H11C_10.70340.17570.29050.039*
C12_10.5723 (3)0.2501 (3)0.2056 (2)0.0192 (8)
N3_10.4793 (2)0.2570 (3)0.16895 (18)0.0215 (8)
C13_10.0698 (3)0.2318 (4)0.0145 (2)0.0296 (10)
H13A_10.00730.20120.00620.044*
H13B_10.06680.30030.04610.044*
H13C_10.11930.17850.05310.044*
C14_10.1152 (3)0.2546 (4)0.0586 (3)0.0225 (9)
N4_10.1527 (3)0.2706 (3)0.1160 (2)0.0295 (9)
C1_20.0642 (3)0.3380 (3)0.8083 (3)0.0215 (10)
H1A_20.01620.35360.80700.026*
H1B_20.06860.32530.74830.026*
C2_20.1396 (3)0.4331 (4)0.8482 (3)0.0231 (10)
H2A_20.11300.50180.81580.028*
H2B_20.13770.44380.90900.028*
C3_20.3376 (3)0.4858 (3)0.8853 (3)0.0235 (10)
H3A_20.33010.50340.94380.028*
H3B_20.32730.55470.85110.028*
C4_20.4537 (3)0.4383 (3)0.8917 (3)0.0199 (10)
H4A_20.45550.40400.83600.024*
H4B_20.51250.49700.90560.024*
C5_20.5761 (3)0.2929 (3)0.9633 (2)0.0213 (9)
H5A_20.61100.27151.02410.026*
H5B_20.63230.33830.94390.026*
C6_20.5499 (3)0.1906 (3)0.9081 (2)0.0210 (10)
H6A_20.51890.21070.84650.025*
H6B_20.62030.14680.91390.025*
C7_20.4366 (3)0.0271 (3)0.8916 (3)0.0203 (10)
H7A_20.49540.02970.91410.024*
H7B_20.42970.03740.82920.024*
C8_20.3237 (3)0.0084 (4)0.9048 (3)0.0230 (10)
H8A_20.31020.08740.89020.028*
H8B_20.32360.00250.96590.028*
C9_20.1281 (3)0.0491 (4)0.8680 (3)0.0232 (11)
H9A_20.13730.05580.93100.028*
H9B_20.09190.02280.84820.028*
C10_20.0553 (3)0.1420 (3)0.8205 (3)0.0204 (10)
H10A_20.05450.14090.75860.024*
H10B_20.02420.13420.82470.024*
O1_20.10401 (19)0.2437 (2)0.86012 (15)0.0200 (6)
O2_20.2525 (2)0.4073 (2)0.84435 (17)0.0201 (7)
O3_20.4759 (2)0.3573 (2)0.95883 (17)0.0190 (6)
O4_20.4682 (2)0.1287 (2)0.93722 (17)0.0194 (7)
O5_20.2366 (2)0.0568 (2)0.84958 (17)0.0203 (7)
Ni2_20.29650 (4)0.22252 (4)0.63415 (3)0.01618 (13)
O6_20.3031 (2)0.2275 (2)0.76117 (16)0.0177 (6)
H6C_20.284 (3)0.1746 (18)0.788 (2)0.027*
H6D_20.280 (3)0.2836 (17)0.782 (2)0.027*
O7_20.2865 (2)0.2124 (2)0.50680 (15)0.0233 (7)
H7C_20.3446 (18)0.203 (3)0.4869 (19)0.035*
H7D_20.2340 (19)0.230 (3)0.4645 (17)0.035*
N1_20.2457 (3)0.4595 (3)0.6422 (2)0.0234 (8)
O8_20.3473 (2)0.4709 (2)0.68356 (16)0.0288 (6)
O9_20.2086 (2)0.3632 (2)0.61173 (15)0.0269 (6)
O10_20.1796 (3)0.5369 (2)0.6298 (2)0.0477 (9)
N2_20.1993 (3)0.0374 (3)0.6218 (2)0.0251 (9)
O11_20.3085 (2)0.0488 (2)0.64360 (18)0.0202 (6)
O12_20.1437 (2)0.1273 (2)0.61016 (16)0.0204 (6)
O13_20.1538 (2)0.0523 (2)0.6131 (2)0.0414 (8)
C11_20.6786 (3)0.2953 (3)0.7514 (2)0.0245 (10)
H11A_20.68310.36790.77900.037*
H11B_20.72890.29360.71280.037*
H11C_20.70250.23860.79600.037*
C12_20.5620 (3)0.2742 (3)0.7019 (2)0.0202 (9)
N3_20.4685 (2)0.2567 (3)0.66560 (18)0.0198 (7)
C13_20.0517 (3)0.2723 (4)0.4996 (3)0.0326 (11)
H13A_20.10390.30840.45000.049*
H13B_20.02510.20260.48080.049*
H13C_20.01400.32040.52350.049*
C14_20.1112 (3)0.2504 (4)0.5658 (3)0.0237 (9)
N4_20.1583 (3)0.2349 (3)0.6170 (2)0.0335 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C1_10.019 (2)0.031 (3)0.020 (3)0.0003 (19)0.0014 (19)0.004 (2)
C2_10.021 (2)0.031 (3)0.024 (3)0.010 (2)0.0112 (19)0.005 (2)
C3_10.032 (3)0.018 (2)0.022 (2)0.0073 (19)0.0022 (19)0.0013 (18)
C4_10.025 (2)0.018 (2)0.021 (2)0.0107 (19)0.0059 (18)0.0011 (19)
C5_10.0122 (19)0.030 (2)0.015 (2)0.0044 (17)0.0024 (16)0.0043 (19)
C6_10.017 (2)0.029 (3)0.014 (2)0.0013 (18)0.0061 (17)0.0002 (19)
C7_10.026 (2)0.024 (2)0.013 (2)0.0015 (19)0.0039 (19)0.0007 (19)
C8_10.027 (2)0.020 (2)0.018 (2)0.0013 (18)0.0043 (19)0.0071 (18)
C9_10.023 (2)0.029 (3)0.020 (2)0.010 (2)0.0119 (19)0.008 (2)
C10_10.014 (2)0.029 (3)0.021 (3)0.0040 (19)0.0015 (19)0.003 (2)
O1_10.0165 (13)0.0242 (17)0.0176 (16)0.0039 (14)0.0024 (11)0.0010 (15)
O2_10.0169 (14)0.0178 (15)0.0219 (16)0.0018 (12)0.0061 (12)0.0049 (12)
O3_10.0220 (15)0.0231 (16)0.0151 (15)0.0051 (12)0.0062 (12)0.0028 (12)
O4_10.0197 (15)0.0217 (16)0.0203 (16)0.0031 (13)0.0069 (13)0.0013 (13)
O5_10.0177 (15)0.0317 (18)0.0157 (16)0.0012 (13)0.0048 (12)0.0037 (14)
Ni1_10.0146 (2)0.0215 (3)0.0128 (3)0.0019 (2)0.0048 (2)0.0002 (2)
O6_10.0230 (13)0.0126 (15)0.0155 (15)0.0026 (13)0.0085 (11)0.0001 (13)
O7_10.0145 (12)0.054 (2)0.0107 (14)0.0032 (14)0.0050 (10)0.0007 (14)
N1_10.028 (2)0.035 (2)0.016 (2)0.0002 (18)0.0108 (16)0.0050 (17)
O8_10.0267 (15)0.0217 (14)0.0306 (15)0.0081 (13)0.0160 (12)0.0066 (12)
O9_10.0260 (15)0.0390 (18)0.0368 (16)0.0058 (14)0.0037 (13)0.0029 (14)
O10_10.0417 (18)0.0198 (17)0.0428 (18)0.0043 (14)0.0200 (15)0.0001 (14)
N2_10.024 (2)0.038 (3)0.0211 (19)0.0114 (18)0.0065 (16)0.0007 (17)
O11_10.0191 (14)0.0203 (14)0.0273 (16)0.0002 (13)0.0078 (12)0.0040 (14)
O12_10.0190 (15)0.0282 (17)0.0285 (16)0.0049 (12)0.0058 (12)0.0055 (13)
O13_10.0424 (19)0.040 (2)0.047 (2)0.0226 (17)0.0040 (16)0.0013 (16)
C11_10.0189 (18)0.038 (3)0.021 (2)0.0018 (18)0.0059 (15)0.0012 (19)
C12_10.0247 (19)0.023 (2)0.0132 (19)0.0019 (18)0.0103 (16)0.0004 (17)
N3_10.0206 (16)0.031 (2)0.0136 (17)0.0002 (17)0.0062 (13)0.0001 (17)
C13_10.029 (2)0.035 (3)0.026 (2)0.002 (2)0.0101 (18)0.004 (2)
C14_10.0122 (18)0.024 (2)0.029 (2)0.0017 (19)0.0012 (17)0.003 (2)
N4_10.0238 (18)0.037 (2)0.030 (2)0.0024 (18)0.0111 (16)0.0018 (19)
C1_20.015 (2)0.028 (2)0.020 (2)0.0038 (18)0.0029 (19)0.001 (2)
C2_20.018 (2)0.023 (3)0.026 (3)0.0062 (19)0.0018 (19)0.001 (2)
C3_20.019 (2)0.021 (2)0.029 (2)0.0021 (18)0.0040 (19)0.0026 (19)
C4_20.017 (2)0.023 (2)0.019 (2)0.0019 (18)0.0040 (18)0.0028 (19)
C5_20.0157 (19)0.028 (2)0.021 (2)0.0022 (18)0.0062 (17)0.0058 (19)
C6_20.019 (2)0.026 (2)0.018 (2)0.0009 (18)0.0045 (17)0.0029 (19)
C7_20.020 (2)0.017 (2)0.023 (2)0.0001 (18)0.0046 (18)0.0013 (19)
C8_20.024 (2)0.020 (2)0.021 (2)0.0024 (18)0.0015 (19)0.0022 (18)
C9_20.021 (2)0.026 (3)0.024 (3)0.004 (2)0.009 (2)0.007 (2)
C10_20.016 (2)0.026 (2)0.021 (2)0.0075 (18)0.0077 (19)0.006 (2)
O1_20.0185 (13)0.0242 (17)0.0146 (15)0.0018 (14)0.0002 (11)0.0002 (14)
O2_20.0157 (15)0.0227 (16)0.0219 (16)0.0027 (12)0.0052 (12)0.0023 (13)
O3_20.0165 (14)0.0210 (15)0.0216 (16)0.0003 (12)0.0090 (12)0.0009 (13)
O4_20.0216 (15)0.0225 (16)0.0159 (16)0.0025 (13)0.0081 (12)0.0015 (13)
O5_20.0174 (15)0.0238 (17)0.0211 (17)0.0013 (13)0.0073 (12)0.0062 (14)
Ni2_20.0153 (2)0.0209 (3)0.0126 (3)0.0020 (2)0.0042 (2)0.0003 (2)
O6_20.0217 (13)0.0210 (16)0.0127 (15)0.0032 (13)0.0084 (11)0.0013 (13)
O7_20.0179 (13)0.0418 (19)0.0109 (14)0.0070 (13)0.0050 (11)0.0012 (13)
N1_20.031 (2)0.021 (2)0.0154 (19)0.0007 (16)0.0022 (16)0.0006 (15)
O8_20.0211 (14)0.0273 (16)0.0358 (16)0.0031 (12)0.0036 (12)0.0031 (13)
O9_20.0319 (16)0.0204 (16)0.0245 (14)0.0003 (12)0.0006 (12)0.0009 (12)
O10_20.0400 (19)0.0223 (18)0.073 (2)0.0163 (15)0.0013 (16)0.0021 (16)
N2_20.025 (2)0.028 (2)0.0221 (19)0.0007 (16)0.0063 (16)0.0006 (16)
O11_20.0137 (13)0.0222 (15)0.0244 (16)0.0033 (12)0.0042 (12)0.0009 (13)
O12_20.0138 (14)0.0245 (16)0.0213 (15)0.0012 (12)0.0021 (12)0.0021 (13)
O13_20.0398 (18)0.0251 (18)0.055 (2)0.0186 (15)0.0055 (15)0.0027 (16)
C11_20.0179 (18)0.035 (3)0.021 (2)0.0015 (17)0.0054 (16)0.0027 (18)
C12_20.0219 (19)0.023 (2)0.018 (2)0.0033 (18)0.0102 (16)0.0021 (18)
N3_20.0234 (16)0.0237 (19)0.0148 (17)0.0015 (16)0.0095 (13)0.0010 (16)
C13_20.024 (2)0.045 (3)0.030 (2)0.003 (2)0.0080 (18)0.009 (2)
C14_20.022 (2)0.023 (2)0.023 (2)0.002 (2)0.0004 (18)0.001 (2)
N4_20.031 (2)0.033 (2)0.037 (2)0.0022 (18)0.0111 (17)0.001 (2)
Geometric parameters (Å, º) top
C1_1—O1_11.442 (5)C1_2—O1_21.423 (5)
C1_1—C2_11.499 (6)C1_2—C2_21.504 (6)
C1_1—H1A_10.9900C1_2—H1A_20.9900
C1_1—H1B_10.9900C1_2—H1B_20.9900
C2_1—O2_11.435 (4)C2_2—O2_21.425 (4)
C2_1—H2A_10.9900C2_2—H2A_20.9900
C2_1—H2B_10.9900C2_2—H2B_20.9900
C3_1—O2_11.426 (4)C3_2—O2_21.429 (4)
C3_1—C4_11.495 (5)C3_2—C4_21.502 (5)
C3_1—H3A_10.9900C3_2—H3A_20.9900
C3_1—H3B_10.9900C3_2—H3B_20.9900
C4_1—O3_11.440 (4)C4_2—O3_21.432 (4)
C4_1—H4A_10.9900C4_2—H4A_20.9900
C4_1—H4B_10.9900C4_2—H4B_20.9900
C5_1—O3_11.427 (4)C5_2—O3_21.432 (4)
C5_1—C6_11.503 (5)C5_2—C6_21.507 (5)
C5_1—H5A_10.9900C5_2—H5A_20.9900
C5_1—H5B_10.9900C5_2—H5B_20.9900
C6_1—O4_11.418 (4)C6_2—O4_21.420 (4)
C6_1—H6A_10.9900C6_2—H6A_20.9900
C6_1—H6B_10.9900C6_2—H6B_20.9900
C7_1—O4_11.425 (5)C7_2—O4_21.431 (4)
C7_1—C8_11.497 (5)C7_2—C8_21.505 (5)
C7_1—H7A_10.9900C7_2—H7A_20.9900
C7_1—H7B_10.9900C7_2—H7B_20.9900
C8_1—O5_11.435 (4)C8_2—O5_21.426 (4)
C8_1—H8A_10.9900C8_2—H8A_20.9900
C8_1—H8B_10.9900C8_2—H8B_20.9900
C9_1—O5_11.430 (4)C9_2—O5_21.428 (4)
C9_1—C10_11.488 (6)C9_2—C10_21.510 (6)
C9_1—H9A_10.9900C9_2—H9A_20.9900
C9_1—H9B_10.9900C9_2—H9B_20.9900
C10_1—O1_11.425 (5)C10_2—O1_21.439 (5)
C10_1—H10A_10.9900C10_2—H10A_20.9900
C10_1—H10B_10.9900C10_2—H10B_20.9900
Ni1_1—O7_12.015 (2)Ni2_2—O9_21.997 (3)
Ni1_1—O6_12.029 (2)Ni2_2—O7_22.017 (2)
Ni1_1—O8_12.046 (3)Ni2_2—O6_22.018 (2)
Ni1_1—N3_12.059 (3)Ni2_2—N3_22.055 (3)
Ni1_1—O11_12.103 (3)Ni2_2—O11_22.117 (2)
Ni1_1—O12_12.137 (3)Ni2_2—O12_22.131 (2)
O6_1—H6C_10.832 (17)O6_2—H6C_20.840 (17)
O6_1—H6D_10.847 (16)O6_2—H6D_20.842 (17)
O7_1—H7C_10.818 (17)O7_2—H7C_20.856 (17)
O7_1—H7D_10.828 (17)O7_2—H7D_20.825 (17)
N1_1—O9_11.241 (4)N1_2—O10_21.218 (4)
N1_1—O10_11.244 (4)N1_2—O8_21.243 (4)
N1_1—O8_11.268 (4)N1_2—O9_21.298 (4)
N2_1—O13_11.230 (4)N2_2—O13_21.211 (4)
N2_1—O12_11.273 (4)N2_2—O12_21.272 (4)
N2_1—O11_11.276 (4)N2_2—O11_21.284 (4)
C11_1—C12_11.462 (5)C11_2—C12_21.449 (5)
C11_1—H11A_10.9800C11_2—H11A_20.9800
C11_1—H11B_10.9800C11_2—H11B_20.9800
C11_1—H11C_10.9800C11_2—H11C_20.9800
C12_1—N3_11.129 (4)C12_2—N3_21.149 (4)
C13_1—C14_11.448 (5)C13_2—C14_21.460 (5)
C13_1—H13A_10.9800C13_2—H13A_20.9800
C13_1—H13B_10.9800C13_2—H13B_20.9800
C13_1—H13C_10.9800C13_2—H13C_20.9800
C14_1—N4_11.147 (4)C14_2—N4_21.136 (4)
O1_1—C1_1—C2_1108.0 (3)O1_2—C1_2—C2_2107.2 (3)
O1_1—C1_1—H1A_1110.1O1_2—C1_2—H1A_2110.3
C2_1—C1_1—H1A_1110.1C2_2—C1_2—H1A_2110.3
O1_1—C1_1—H1B_1110.1O1_2—C1_2—H1B_2110.3
C2_1—C1_1—H1B_1110.1C2_2—C1_2—H1B_2110.3
H1A_1—C1_1—H1B_1108.4H1A_2—C1_2—H1B_2108.5
O2_1—C2_1—C1_1107.3 (3)O2_2—C2_2—C1_2107.2 (3)
O2_1—C2_1—H2A_1110.3O2_2—C2_2—H2A_2110.3
C1_1—C2_1—H2A_1110.3C1_2—C2_2—H2A_2110.3
O2_1—C2_1—H2B_1110.3O2_2—C2_2—H2B_2110.3
C1_1—C2_1—H2B_1110.3C1_2—C2_2—H2B_2110.3
H2A_1—C2_1—H2B_1108.5H2A_2—C2_2—H2B_2108.5
O2_1—C3_1—C4_1108.7 (3)O2_2—C3_2—C4_2109.0 (3)
O2_1—C3_1—H3A_1109.9O2_2—C3_2—H3A_2109.9
C4_1—C3_1—H3A_1109.9C4_2—C3_2—H3A_2109.9
O2_1—C3_1—H3B_1109.9O2_2—C3_2—H3B_2109.9
C4_1—C3_1—H3B_1109.9C4_2—C3_2—H3B_2109.9
H3A_1—C3_1—H3B_1108.3H3A_2—C3_2—H3B_2108.3
O3_1—C4_1—C3_1108.6 (3)O3_2—C4_2—C3_2107.5 (3)
O3_1—C4_1—H4A_1110.0O3_2—C4_2—H4A_2110.2
C3_1—C4_1—H4A_1110.0C3_2—C4_2—H4A_2110.2
O3_1—C4_1—H4B_1110.0O3_2—C4_2—H4B_2110.2
C3_1—C4_1—H4B_1110.0C3_2—C4_2—H4B_2110.2
H4A_1—C4_1—H4B_1108.4H4A_2—C4_2—H4B_2108.5
O3_1—C5_1—C6_1112.3 (3)O3_2—C5_2—C6_2112.2 (3)
O3_1—C5_1—H5A_1109.1O3_2—C5_2—H5A_2109.2
C6_1—C5_1—H5A_1109.1C6_2—C5_2—H5A_2109.2
O3_1—C5_1—H5B_1109.1O3_2—C5_2—H5B_2109.2
C6_1—C5_1—H5B_1109.1C6_2—C5_2—H5B_2109.2
H5A_1—C5_1—H5B_1107.9H5A_2—C5_2—H5B_2107.9
O4_1—C6_1—C5_1107.2 (3)O4_2—C6_2—C5_2107.4 (3)
O4_1—C6_1—H6A_1110.3O4_2—C6_2—H6A_2110.2
C5_1—C6_1—H6A_1110.3C5_2—C6_2—H6A_2110.2
O4_1—C6_1—H6B_1110.3O4_2—C6_2—H6B_2110.2
C5_1—C6_1—H6B_1110.3C5_2—C6_2—H6B_2110.2
H6A_1—C6_1—H6B_1108.5H6A_2—C6_2—H6B_2108.5
O4_1—C7_1—C8_1107.2 (3)O4_2—C7_2—C8_2107.7 (3)
O4_1—C7_1—H7A_1110.3O4_2—C7_2—H7A_2110.2
C8_1—C7_1—H7A_1110.3C8_2—C7_2—H7A_2110.2
O4_1—C7_1—H7B_1110.3O4_2—C7_2—H7B_2110.2
C8_1—C7_1—H7B_1110.3C8_2—C7_2—H7B_2110.2
H7A_1—C7_1—H7B_1108.5H7A_2—C7_2—H7B_2108.5
O5_1—C8_1—C7_1108.0 (3)O5_2—C8_2—C7_2107.8 (3)
O5_1—C8_1—H8A_1110.1O5_2—C8_2—H8A_2110.1
C7_1—C8_1—H8A_1110.1C7_2—C8_2—H8A_2110.1
O5_1—C8_1—H8B_1110.1O5_2—C8_2—H8B_2110.1
C7_1—C8_1—H8B_1110.1C7_2—C8_2—H8B_2110.1
H8A_1—C8_1—H8B_1108.4H8A_2—C8_2—H8B_2108.5
O5_1—C9_1—C10_1107.4 (3)O5_2—C9_2—C10_2107.1 (3)
O5_1—C9_1—H9A_1110.2O5_2—C9_2—H9A_2110.3
C10_1—C9_1—H9A_1110.2C10_2—C9_2—H9A_2110.3
O5_1—C9_1—H9B_1110.2O5_2—C9_2—H9B_2110.3
C10_1—C9_1—H9B_1110.2C10_2—C9_2—H9B_2110.3
H9A_1—C9_1—H9B_1108.5H9A_2—C9_2—H9B_2108.5
O1_1—C10_1—C9_1107.6 (3)O1_2—C10_2—C9_2107.6 (3)
O1_1—C10_1—H10A_1110.2O1_2—C10_2—H10A_2110.2
C9_1—C10_1—H10A_1110.2C9_2—C10_2—H10A_2110.2
O1_1—C10_1—H10B_1110.2O1_2—C10_2—H10B_2110.2
C9_1—C10_1—H10B_1110.2C9_2—C10_2—H10B_2110.2
H10A_1—C10_1—H10B_1108.5H10A_2—C10_2—H10B_2108.5
C10_1—O1_1—C1_1113.0 (3)C1_2—O1_2—C10_2113.4 (3)
C3_1—O2_1—C2_1114.1 (3)C2_2—O2_2—C3_2114.8 (3)
C5_1—O3_1—C4_1115.2 (3)C4_2—O3_2—C5_2113.6 (3)
C6_1—O4_1—C7_1113.4 (3)C6_2—O4_2—C7_2113.8 (3)
C9_1—O5_1—C8_1114.9 (3)C8_2—O5_2—C9_2114.0 (3)
O7_1—Ni1_1—O6_1176.58 (10)O9_2—Ni2_2—O7_289.04 (11)
O7_1—Ni1_1—O8_193.05 (12)O9_2—Ni2_2—O6_291.93 (10)
O6_1—Ni1_1—O8_186.67 (10)O7_2—Ni2_2—O6_2177.88 (11)
O7_1—Ni1_1—N3_192.70 (10)O9_2—Ni2_2—N3_2109.37 (13)
O6_1—Ni1_1—N3_190.67 (11)O7_2—Ni2_2—N3_292.47 (10)
O8_1—Ni1_1—N3_184.90 (13)O6_2—Ni2_2—N3_288.99 (11)
O7_1—Ni1_1—O11_192.48 (13)O9_2—Ni2_2—O11_2152.77 (11)
O6_1—Ni1_1—O11_187.75 (11)O7_2—Ni2_2—O11_289.89 (12)
O8_1—Ni1_1—O11_1174.39 (10)O6_2—Ni2_2—O11_288.39 (12)
N3_1—Ni1_1—O11_195.76 (13)N3_2—Ni2_2—O11_297.87 (13)
O7_1—Ni1_1—O12_189.17 (11)O9_2—Ni2_2—O12_291.87 (11)
O6_1—Ni1_1—O12_187.95 (10)O7_2—Ni2_2—O12_288.33 (10)
O8_1—Ni1_1—O12_1117.69 (10)O6_2—Ni2_2—O12_289.75 (10)
N3_1—Ni1_1—O12_1157.23 (13)N3_2—Ni2_2—O12_2158.75 (13)
O11_1—Ni1_1—O12_161.47 (10)O11_2—Ni2_2—O12_260.90 (10)
Ni1_1—O6_1—H6C_1109 (2)Ni2_2—O6_2—H6C_2124 (3)
Ni1_1—O6_1—H6D_1130 (2)Ni2_2—O6_2—H6D_2120 (3)
H6C_1—O6_1—H6D_1104 (2)H6C_2—O6_2—H6D_2104 (2)
Ni1_1—O7_1—H7C_1122 (2)Ni2_2—O7_2—H7C_2124 (2)
Ni1_1—O7_1—H7D_1129 (2)Ni2_2—O7_2—H7D_2130 (2)
H7C_1—O7_1—H7D_1109 (3)H7C_2—O7_2—H7D_2105 (2)
O9_1—N1_1—O10_1119.7 (4)O10_2—N1_2—O8_2121.3 (4)
O9_1—N1_1—O8_1120.2 (4)O10_2—N1_2—O9_2119.0 (3)
O10_1—N1_1—O8_1120.0 (3)O8_2—N1_2—O9_2119.7 (3)
N1_1—O8_1—Ni1_1120.7 (2)N1_2—O9_2—Ni2_2125.9 (2)
O13_1—N2_1—O12_1121.9 (3)O13_2—N2_2—O12_2123.1 (3)
O13_1—N2_1—O11_1121.6 (4)O13_2—N2_2—O11_2122.2 (4)
O12_1—N2_1—O11_1116.5 (3)O12_2—N2_2—O11_2114.7 (3)
N2_1—O11_1—Ni1_191.8 (2)N2_2—O11_2—Ni2_292.3 (2)
N2_1—O12_1—Ni1_190.3 (2)N2_2—O12_2—Ni2_292.0 (2)
C12_1—C11_1—H11A_1109.5C12_2—C11_2—H11A_2109.5
C12_1—C11_1—H11B_1109.5C12_2—C11_2—H11B_2109.5
H11A_1—C11_1—H11B_1109.5H11A_2—C11_2—H11B_2109.5
C12_1—C11_1—H11C_1109.5C12_2—C11_2—H11C_2109.5
H11A_1—C11_1—H11C_1109.5H11A_2—C11_2—H11C_2109.5
H11B_1—C11_1—H11C_1109.5H11B_2—C11_2—H11C_2109.5
N3_1—C12_1—C11_1178.4 (4)N3_2—C12_2—C11_2177.4 (4)
C12_1—N3_1—Ni1_1164.2 (3)C12_2—N3_2—Ni2_2164.4 (3)
C14_1—C13_1—H13A_1109.5C14_2—C13_2—H13A_2109.5
C14_1—C13_1—H13B_1109.5C14_2—C13_2—H13B_2109.5
H13A_1—C13_1—H13B_1109.5H13A_2—C13_2—H13B_2109.5
C14_1—C13_1—H13C_1109.5C14_2—C13_2—H13C_2109.5
H13A_1—C13_1—H13C_1109.5H13A_2—C13_2—H13C_2109.5
H13B_1—C13_1—H13C_1109.5H13B_2—C13_2—H13C_2109.5
N4_1—C14_1—C13_1178.5 (5)N4_2—C14_2—C13_2179.0 (5)
O1_1—C1_1—C2_1—O2_161.0 (4)O2_2—C3_2—C4_2—O3_274.4 (4)
O2_1—C3_1—C4_1—O3_171.7 (4)O3_2—C5_2—C6_2—O4_258.2 (4)
O3_1—C5_1—C6_1—O4_158.8 (4)O4_2—C7_2—C8_2—O5_277.2 (4)
O4_1—C7_1—C8_1—O5_179.6 (4)O5_2—C9_2—C10_2—O1_267.6 (4)
O5_1—C9_1—C10_1—O1_168.6 (4)C2_2—C1_2—O1_2—C10_2168.2 (3)
C9_1—C10_1—O1_1—C1_1166.0 (3)C9_2—C10_2—O1_2—C1_2163.7 (3)
C2_1—C1_1—O1_1—C10_1166.9 (3)C1_2—C2_2—O2_2—C3_2175.8 (3)
C4_1—C3_1—O2_1—C2_1167.0 (3)C4_2—C3_2—O2_2—C2_2169.1 (3)
C1_1—C2_1—O2_1—C3_1176.2 (3)C3_2—C4_2—O3_2—C5_2170.8 (3)
C6_1—C5_1—O3_1—C4_191.2 (4)C6_2—C5_2—O3_2—C4_290.4 (4)
C3_1—C4_1—O3_1—C5_1171.4 (3)C5_2—C6_2—O4_2—C7_2178.8 (3)
C5_1—C6_1—O4_1—C7_1179.8 (3)C8_2—C7_2—O4_2—C6_2159.8 (3)
C8_1—C7_1—O4_1—C6_1160.6 (3)C7_2—C8_2—O5_2—C9_2167.4 (3)
C10_1—C9_1—O5_1—C8_1163.5 (3)C10_2—C9_2—O5_2—C8_2166.2 (3)
C7_1—C8_1—O5_1—C9_1166.7 (3)O10_2—N1_2—O9_2—Ni2_2173.4 (3)
O9_1—N1_1—O8_1—Ni1_18.5 (4)O8_2—N1_2—O9_2—Ni2_26.4 (5)
O10_1—N1_1—O8_1—Ni1_1169.1 (3)O7_2—Ni2_2—O9_2—N1_2116.8 (3)
O7_1—Ni1_1—O8_1—N1_192.4 (3)O6_2—Ni2_2—O9_2—N1_265.1 (3)
O6_1—Ni1_1—O8_1—N1_184.2 (3)N3_2—Ni2_2—O9_2—N1_224.5 (3)
N3_1—Ni1_1—O8_1—N1_1175.1 (3)O11_2—Ni2_2—O9_2—N1_2155.3 (3)
O12_1—Ni1_1—O8_1—N1_11.7 (3)O12_2—Ni2_2—O9_2—N1_2154.9 (3)
O13_1—N2_1—O11_1—Ni1_1178.1 (4)O13_2—N2_2—O11_2—Ni2_2177.3 (4)
O12_1—N2_1—O11_1—Ni1_11.4 (4)O12_2—N2_2—O11_2—Ni2_22.6 (3)
O7_1—Ni1_1—O11_1—N2_188.6 (2)O9_2—Ni2_2—O11_2—N2_21.2 (4)
O6_1—Ni1_1—O11_1—N2_188.0 (2)O7_2—Ni2_2—O11_2—N2_286.5 (2)
N3_1—Ni1_1—O11_1—N2_1178.5 (2)O6_2—Ni2_2—O11_2—N2_292.2 (2)
O12_1—Ni1_1—O11_1—N2_10.9 (2)N3_2—Ni2_2—O11_2—N2_2179.0 (2)
O13_1—N2_1—O12_1—Ni1_1178.2 (4)O12_2—Ni2_2—O11_2—N2_21.6 (2)
O11_1—N2_1—O12_1—Ni1_11.4 (4)O13_2—N2_2—O12_2—Ni2_2177.3 (4)
O7_1—Ni1_1—O12_1—N2_194.2 (2)O11_2—N2_2—O12_2—Ni2_22.6 (3)
O6_1—Ni1_1—O12_1—N2_187.7 (2)O9_2—Ni2_2—O12_2—N2_2178.1 (2)
O8_1—Ni1_1—O12_1—N2_1172.8 (2)O7_2—Ni2_2—O12_2—N2_289.2 (2)
N3_1—Ni1_1—O12_1—N2_10.8 (4)O6_2—Ni2_2—O12_2—N2_289.9 (2)
O11_1—Ni1_1—O12_1—N2_10.9 (2)N3_2—Ni2_2—O12_2—N2_23.4 (4)
O7_1—Ni1_1—N3_1—C12_1173.1 (14)O11_2—Ni2_2—O12_2—N2_21.6 (2)
O6_1—Ni1_1—N3_1—C12_16.3 (14)O9_2—Ni2_2—N3_2—C12_295.4 (13)
O8_1—Ni1_1—N3_1—C12_180.2 (14)O7_2—Ni2_2—N3_2—C12_2174.8 (13)
O11_1—Ni1_1—N3_1—C12_194.2 (14)O6_2—Ni2_2—N3_2—C12_23.7 (13)
O12_1—Ni1_1—N3_1—C12_192.6 (14)O11_2—Ni2_2—N3_2—C12_284.5 (13)
O1_2—C1_2—C2_2—O2_262.5 (4)O12_2—Ni2_2—N3_2—C12_283.0 (14)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6_1—H6C_1···O2_10.83 (2)1.89 (2)2.695 (4)164 (3)
O6_1—H6D_1···O5_10.85 (2)1.94 (2)2.756 (4)161 (3)
O7_1—H7C_1···O3_2i0.82 (2)2.04 (2)2.810 (3)157 (4)
O7_1—H7D_1···O1_2i0.83 (2)2.01 (2)2.830 (3)173 (4)
O6_2—H6C_2···O5_20.84 (2)1.91 (2)2.752 (4)178 (3)
O6_2—H6D_2···O2_20.84 (2)1.88 (2)2.710 (4)170 (4)
O7_2—H7C_2···O3_10.86 (2)1.93 (2)2.758 (4)161 (4)
O7_2—H7D_2···O1_10.83 (2)2.02 (2)2.841 (3)172 (4)
Symmetry code: (i) x, y, z1.
(6) top
Crystal data top
C10H24O7Ni2+·2(NO3)F(000) = 2760
Mr = 439.02Dx = 1.682 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 12375 reflections
a = 14.676 (1) Åθ = 1.0–27.5°
b = 13.961 (1) ŵ = 1.19 mm1
c = 25.552 (2) ÅT = 90 K
β = 96.56 (1)°Block, pale yellow
V = 5201.1 (7) Å30.40 × 0.15 × 0.10 mm
Z = 12
Data collection top
Nonius KappaCCD
diffractometer
11918 independent reflections
Radiation source: fine-focus sealed tube6757 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.038
Detector resolution: 18 pixels mm-1θmax = 27.5°, θmin = 1.4°
ω scans at fixed χ = 55°h = 1919
Absorption correction: multi-scan
Scalepack (Otwinowski & Minor, 2006)
k = 1818
Tmin = 0.647, Tmax = 0.890l = 3333
23212 measured reflections
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)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.102H atoms treated by a mixture of independent and constrained refinement
S = 0.96 w = 1/[σ2(Fo2) + (0.0457P)2]
where P = (Fo2 + 2Fc2)/3
11918 reflections(Δ/σ)max = 0.002
751 parametersΔρmax = 0.42 e Å3
18 restraintsΔρmin = 0.56 e Å3
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.

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni1_10.2459 (2)0.4976 (2)0.01306 (13)0.0149 (3)0.333 (6)
Ni1'_10.27083 (19)0.50958 (13)0.00981 (6)0.0149 (3)0.667 (6)
O1_10.38339 (9)0.53232 (10)0.03377 (5)0.0157 (3)
O2_10.34722 (9)0.60436 (10)0.05823 (5)0.0174 (4)
O3_10.20278 (9)0.51376 (10)0.08610 (5)0.0188 (4)
O4_10.11275 (10)0.43362 (10)0.00102 (5)0.0208 (4)
O5_10.23707 (9)0.43487 (10)0.06388 (5)0.0170 (3)
O6_10.32115 (12)0.38483 (11)0.03858 (6)0.0270 (4)
H6W1_10.3383 (16)0.3446 (13)0.0178 (6)0.040*
H6W2_10.3421 (15)0.3701 (16)0.0682 (4)0.040*
O7_10.20386 (11)0.62269 (11)0.02049 (6)0.0245 (4)
H7W1_10.1841 (15)0.6703 (12)0.0060 (7)0.037*
H7W2_10.1697 (13)0.6159 (15)0.0491 (5)0.037*
C1_10.43095 (14)0.61736 (15)0.01440 (8)0.0199 (5)
H1A_10.39600.67520.02690.024*
H1B_10.49240.62040.02680.024*
C2_10.43941 (14)0.61124 (16)0.04465 (8)0.0208 (5)
H2A_10.47550.55410.05720.025*
H2B_10.47010.66900.06070.025*
C3_10.34042 (14)0.59448 (16)0.11375 (8)0.0191 (5)
H3A_10.37010.64920.13360.023*
H3B_10.37000.53440.12750.023*
C4_10.23920 (14)0.59258 (15)0.11840 (8)0.0190 (5)
H4A_10.22800.58270.15550.023*
H4B_10.21010.65360.10570.023*
C5_10.10368 (14)0.50691 (16)0.08103 (8)0.0226 (6)
H5A_10.07550.56410.06290.027*
H5B_10.08180.50180.11620.027*
C6_10.07930 (15)0.41826 (17)0.04911 (8)0.0245 (6)
H6A_10.10870.36120.06680.029*
H6B_10.01200.40850.04450.029*
C7_10.11802 (15)0.34817 (15)0.03170 (8)0.0208 (5)
H7A_10.05620.32030.04080.025*
H7B_10.15750.30000.01180.025*
C8_10.15841 (14)0.37754 (16)0.08085 (8)0.0205 (5)
H8A_10.17640.32040.10020.025*
H8B_10.11330.41490.10440.025*
C9_10.30343 (14)0.44133 (15)0.10078 (8)0.0174 (5)
H9A_10.27260.44060.13730.021*
H9B_10.34660.38670.09630.021*
C10_10.35397 (14)0.53437 (15)0.08964 (8)0.0173 (5)
H10A_10.40730.53870.11000.021*
H10B_10.31300.58970.09880.021*
Ni2_20.26091 (16)0.5013 (2)0.32716 (13)0.0148 (3)0.435 (4)
Ni2'_20.23445 (17)0.49127 (17)0.32948 (9)0.0148 (3)0.565 (4)
O1_20.11725 (9)0.47590 (10)0.36888 (5)0.0177 (4)
O2_20.15809 (9)0.39734 (10)0.27946 (5)0.0185 (4)
O3_20.30631 (10)0.48202 (10)0.25346 (5)0.0190 (4)
O4_20.39393 (10)0.56151 (10)0.34150 (5)0.0187 (4)
O5_20.26889 (10)0.56265 (10)0.40375 (5)0.0186 (4)
O6_20.19608 (11)0.61931 (11)0.29929 (6)0.0253 (4)
H6W1_20.1779 (14)0.6592 (14)0.3198 (6)0.038*
H6W2_20.1597 (13)0.6207 (16)0.2720 (5)0.038*
O7_20.29764 (11)0.37620 (11)0.36100 (6)0.0241 (4)
H7W1_20.3375 (12)0.3800 (15)0.3870 (6)0.036*
H7W2_20.3096 (14)0.3265 (11)0.3453 (7)0.036*
C1_20.06853 (15)0.39101 (16)0.34966 (8)0.0217 (5)
H1A_20.00580.39070.36040.026*
H1B_20.10110.33280.36390.026*
C2_20.06484 (14)0.39381 (16)0.29070 (8)0.0221 (6)
H2A_20.03390.33590.27490.026*
H2B_20.03090.45110.27640.026*
C3_20.16862 (14)0.40189 (16)0.22431 (8)0.0195 (5)
H3A_20.13970.46060.20830.023*
H3B_20.14000.34550.20560.023*
C4_20.27017 (14)0.40298 (15)0.22141 (8)0.0200 (5)
H4A_20.29820.34200.23490.024*
H4B_20.28320.41160.18450.024*
C5_20.40499 (14)0.48708 (16)0.25993 (8)0.0213 (5)
H5A_20.42860.49150.22520.026*
H5B_20.43150.42940.27840.026*
C6_20.42962 (15)0.57516 (16)0.29189 (8)0.0222 (6)
H6A_20.49700.58350.29740.027*
H6B_20.40200.63260.27370.027*
C7_20.39129 (15)0.64686 (15)0.37208 (8)0.0208 (5)
H7A_20.35420.69670.35200.025*
H7B_20.45400.67200.38170.025*
C8_20.34821 (14)0.61927 (15)0.42084 (8)0.0211 (5)
H8A_20.39210.58190.44510.025*
H8B_20.33040.67730.43950.025*
C9_20.19747 (14)0.56401 (15)0.43745 (8)0.0187 (5)
H9A_20.15900.62200.43070.022*
H9B_20.22380.56400.47490.022*
C10_20.14127 (15)0.47525 (16)0.42501 (8)0.0208 (5)
H10A_20.17730.41730.43600.025*
H10B_20.08540.47630.44340.025*
Ni3_30.25743 (18)0.5070 (2)0.65864 (14)0.0141 (3)0.402 (5)
Ni3'_30.23321 (17)0.49364 (16)0.66117 (8)0.0141 (3)0.598 (5)
O1_30.12139 (9)0.46825 (10)0.70640 (5)0.0179 (4)
O2_30.16238 (9)0.39354 (10)0.61585 (5)0.0185 (4)
O3_30.29852 (9)0.49368 (10)0.58486 (5)0.0186 (4)
O4_30.38489 (10)0.58417 (11)0.66884 (6)0.0226 (4)
O5_30.26557 (10)0.56999 (10)0.73541 (5)0.0188 (4)
O6_30.17382 (12)0.61187 (11)0.63074 (6)0.0238 (4)
H6W1_30.1580 (16)0.6555 (12)0.6499 (6)0.036*
H6W2_30.1673 (16)0.6326 (14)0.6002 (4)0.036*
O7_30.31191 (12)0.38859 (12)0.69242 (6)0.0291 (4)
H7W1_30.3292 (15)0.3398 (12)0.6780 (8)0.044*
H7W2_30.3450 (14)0.3963 (16)0.7205 (6)0.044*
C1_30.07827 (16)0.37967 (16)0.68855 (8)0.0247 (6)
H1A_30.01700.37410.70090.030*
H1B_30.11610.32440.70220.030*
C2_30.06993 (15)0.38216 (17)0.62929 (8)0.0250 (6)
H2A_30.04260.32190.61430.030*
H2B_30.03090.43650.61550.030*
C3_30.16820 (14)0.39961 (16)0.56014 (8)0.0211 (5)
H3A_30.13350.45560.54470.025*
H3B_30.14340.34090.54200.025*
C4_30.26893 (14)0.41025 (15)0.55509 (8)0.0194 (5)
H4A_30.30310.35310.56930.023*
H4B_30.27900.41830.51770.023*
C5_30.39475 (14)0.51429 (17)0.58600 (9)0.0246 (6)
H5A_30.41120.52340.54980.030*
H5B_30.43190.46100.60280.030*
C6_30.41152 (16)0.60431 (17)0.61742 (8)0.0275 (6)
H6A_30.47710.62240.62010.033*
H6B_30.37450.65760.60060.033*
C7_30.37453 (15)0.66782 (15)0.70005 (8)0.0215 (5)
H7A_30.32980.71250.68120.026*
H7B_30.43400.70130.70780.026*
C8_30.34055 (15)0.63363 (16)0.75018 (8)0.0226 (6)
H8A_30.39010.59980.77240.027*
H8B_30.32000.68860.77030.027*
C9_30.19840 (14)0.56443 (15)0.77174 (8)0.0170 (5)
H9A_30.15430.61810.76590.020*
H9B_30.22830.56780.80840.020*
C10_30.14982 (15)0.47033 (16)0.76211 (8)0.0193 (5)
H10A_30.19160.41630.77260.023*
H10B_30.09610.46640.78220.023*
N1_40.10425 (12)0.68157 (13)0.14161 (7)0.0174 (4)
O8_40.10097 (10)0.60490 (10)0.11575 (6)0.0216 (4)
O9_40.17420 (11)0.73466 (11)0.13243 (6)0.0260 (4)
O10_40.04194 (10)0.70379 (11)0.17607 (6)0.0289 (4)
N2_50.07968 (12)0.68843 (13)0.18278 (7)0.0180 (4)
O8_50.06941 (10)0.61548 (11)0.21104 (6)0.0246 (4)
O9_50.14205 (10)0.74729 (10)0.19845 (5)0.0231 (4)
O10_50.03073 (10)0.70053 (11)0.14086 (6)0.0276 (4)
N3_60.08160 (13)0.68713 (13)0.51131 (7)0.0186 (4)
O8_60.04813 (11)0.61068 (11)0.52497 (7)0.0364 (5)
O9_60.15743 (10)0.71575 (11)0.53537 (6)0.0249 (4)
O10_60.04359 (10)0.73542 (11)0.47444 (6)0.0263 (4)
N4_70.42588 (12)0.30854 (13)0.15752 (7)0.0177 (4)
O8_70.45472 (12)0.38145 (11)0.13683 (7)0.0378 (5)
O9_70.35490 (10)0.26772 (12)0.13532 (6)0.0291 (4)
O10_70.46409 (10)0.27645 (11)0.19949 (6)0.0271 (4)
N5_80.40805 (12)0.31679 (13)0.48085 (7)0.0164 (4)
O8_80.41209 (10)0.39040 (10)0.45265 (6)0.0221 (4)
O9_80.34480 (10)0.25679 (11)0.46855 (6)0.0240 (4)
O10_80.46365 (10)0.30401 (11)0.52035 (6)0.0280 (4)
N6_90.39680 (12)0.32119 (13)0.81302 (7)0.0178 (4)
O8_90.41368 (10)0.39747 (11)0.78925 (6)0.0251 (4)
O9_90.31868 (10)0.28326 (10)0.80277 (5)0.0215 (4)
O10_90.45461 (10)0.28541 (11)0.84637 (6)0.0253 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni1_10.0160 (8)0.0142 (4)0.0144 (2)0.0024 (5)0.0013 (4)0.0001 (2)
Ni1'_10.0160 (8)0.0142 (4)0.0144 (2)0.0024 (5)0.0013 (4)0.0001 (2)
O1_10.0170 (8)0.0166 (9)0.0135 (7)0.0025 (7)0.0011 (6)0.0002 (7)
O2_10.0171 (8)0.0199 (9)0.0152 (8)0.0024 (7)0.0025 (7)0.0007 (7)
O3_10.0170 (8)0.0198 (9)0.0195 (8)0.0010 (7)0.0014 (7)0.0046 (7)
O4_10.0243 (9)0.0214 (9)0.0176 (8)0.0044 (7)0.0059 (7)0.0025 (7)
O5_10.0158 (8)0.0205 (9)0.0149 (8)0.0034 (7)0.0030 (7)0.0029 (7)
O6_10.0460 (11)0.0199 (10)0.0140 (8)0.0159 (8)0.0015 (8)0.0013 (7)
O7_10.0308 (10)0.0216 (10)0.0189 (9)0.0127 (8)0.0063 (7)0.0038 (7)
C1_10.0187 (13)0.0172 (13)0.0245 (13)0.0038 (11)0.0051 (10)0.0011 (10)
C2_10.0162 (13)0.0218 (14)0.0249 (13)0.0019 (11)0.0044 (10)0.0055 (11)
C3_10.0244 (13)0.0186 (13)0.0141 (11)0.0017 (11)0.0012 (10)0.0047 (10)
C4_10.0245 (13)0.0167 (13)0.0162 (11)0.0027 (10)0.0039 (10)0.0037 (10)
C5_10.0179 (13)0.0308 (15)0.0201 (12)0.0004 (11)0.0058 (10)0.0022 (11)
C6_10.0230 (13)0.0320 (15)0.0199 (12)0.0077 (11)0.0086 (11)0.0011 (11)
C7_10.0214 (13)0.0153 (13)0.0254 (13)0.0058 (10)0.0010 (11)0.0038 (11)
C8_10.0223 (13)0.0191 (13)0.0193 (12)0.0043 (11)0.0013 (10)0.0050 (10)
C9_10.0203 (13)0.0185 (13)0.0135 (11)0.0009 (10)0.0030 (10)0.0020 (10)
C10_10.0186 (13)0.0200 (13)0.0138 (11)0.0009 (11)0.0038 (10)0.0028 (10)
Ni2_20.0152 (9)0.0129 (5)0.0163 (3)0.0009 (6)0.0015 (6)0.0010 (3)
Ni2'_20.0152 (9)0.0129 (5)0.0163 (3)0.0009 (6)0.0015 (6)0.0010 (3)
O1_20.0194 (9)0.0190 (9)0.0146 (8)0.0026 (7)0.0006 (7)0.0008 (7)
O2_20.0182 (9)0.0214 (9)0.0163 (8)0.0005 (7)0.0031 (7)0.0011 (7)
O3_20.0172 (9)0.0186 (9)0.0209 (8)0.0006 (7)0.0007 (7)0.0052 (7)
O4_20.0219 (9)0.0181 (9)0.0166 (8)0.0027 (7)0.0038 (7)0.0013 (7)
O5_20.0175 (8)0.0203 (9)0.0185 (8)0.0044 (7)0.0045 (7)0.0052 (7)
O6_20.0395 (11)0.0194 (10)0.0160 (9)0.0116 (8)0.0011 (8)0.0016 (7)
O7_20.0359 (11)0.0150 (9)0.0189 (9)0.0111 (8)0.0074 (8)0.0037 (7)
C1_20.0202 (13)0.0202 (14)0.0247 (13)0.0040 (11)0.0024 (10)0.0000 (11)
C2_20.0193 (13)0.0262 (14)0.0208 (12)0.0042 (11)0.0029 (10)0.0009 (11)
C3_20.0265 (13)0.0181 (13)0.0135 (11)0.0030 (11)0.0001 (10)0.0045 (10)
C4_20.0259 (14)0.0180 (13)0.0158 (11)0.0034 (11)0.0013 (10)0.0019 (10)
C5_20.0177 (13)0.0261 (14)0.0205 (12)0.0013 (11)0.0038 (10)0.0022 (11)
C6_20.0214 (13)0.0266 (15)0.0198 (12)0.0026 (11)0.0069 (10)0.0014 (11)
C7_20.0227 (13)0.0184 (13)0.0213 (12)0.0047 (11)0.0022 (10)0.0035 (10)
C8_20.0203 (13)0.0191 (13)0.0232 (13)0.0059 (11)0.0001 (10)0.0032 (11)
C9_20.0206 (13)0.0222 (14)0.0143 (11)0.0025 (11)0.0065 (10)0.0005 (10)
C10_20.0234 (13)0.0261 (14)0.0127 (11)0.0030 (11)0.0017 (10)0.0021 (10)
Ni3_30.0146 (8)0.0126 (6)0.0152 (3)0.0000 (5)0.0018 (6)0.0006 (3)
Ni3'_30.0146 (8)0.0126 (6)0.0152 (3)0.0000 (5)0.0018 (6)0.0006 (3)
O1_30.0198 (9)0.0168 (9)0.0164 (8)0.0037 (7)0.0008 (7)0.0017 (7)
O2_30.0175 (8)0.0198 (9)0.0189 (8)0.0009 (7)0.0047 (7)0.0002 (7)
O3_30.0161 (8)0.0223 (9)0.0172 (8)0.0014 (7)0.0003 (7)0.0033 (7)
O4_30.0260 (9)0.0247 (10)0.0180 (8)0.0027 (8)0.0060 (7)0.0030 (7)
O5_30.0182 (8)0.0224 (9)0.0160 (8)0.0050 (7)0.0029 (7)0.0041 (7)
O6_30.0394 (11)0.0191 (10)0.0129 (8)0.0127 (8)0.0026 (8)0.0000 (7)
O7_30.0399 (11)0.0255 (11)0.0201 (9)0.0160 (9)0.0039 (8)0.0008 (8)
C1_30.0248 (14)0.0220 (14)0.0283 (14)0.0057 (11)0.0080 (11)0.0066 (11)
C2_30.0227 (14)0.0263 (15)0.0269 (13)0.0073 (11)0.0061 (11)0.0093 (11)
C3_30.0264 (14)0.0217 (14)0.0147 (12)0.0006 (11)0.0010 (10)0.0060 (10)
C4_30.0267 (14)0.0179 (13)0.0134 (11)0.0059 (11)0.0019 (10)0.0025 (10)
C5_30.0189 (13)0.0337 (16)0.0217 (12)0.0042 (11)0.0037 (10)0.0025 (11)
C6_30.0245 (14)0.0381 (16)0.0212 (13)0.0104 (12)0.0087 (11)0.0016 (12)
C7_30.0241 (13)0.0194 (13)0.0215 (12)0.0064 (11)0.0049 (10)0.0050 (10)
C8_30.0225 (13)0.0245 (14)0.0206 (12)0.0066 (11)0.0009 (10)0.0051 (11)
C9_30.0208 (13)0.0191 (13)0.0116 (11)0.0026 (10)0.0038 (10)0.0013 (10)
C10_30.0237 (14)0.0204 (13)0.0137 (11)0.0018 (11)0.0024 (10)0.0037 (10)
N1_40.0218 (11)0.0163 (11)0.0144 (10)0.0023 (9)0.0035 (9)0.0025 (9)
O8_40.0290 (9)0.0154 (9)0.0200 (8)0.0032 (7)0.0014 (7)0.0055 (7)
O9_40.0332 (10)0.0223 (10)0.0214 (9)0.0110 (8)0.0009 (7)0.0018 (7)
O10_40.0274 (9)0.0328 (11)0.0242 (9)0.0117 (8)0.0065 (8)0.0030 (8)
N2_50.0201 (11)0.0150 (11)0.0194 (10)0.0031 (9)0.0040 (9)0.0021 (9)
O8_50.0305 (10)0.0173 (9)0.0265 (9)0.0033 (8)0.0059 (8)0.0035 (7)
O9_50.0302 (10)0.0176 (9)0.0205 (9)0.0103 (8)0.0015 (7)0.0014 (7)
O10_50.0292 (9)0.0253 (10)0.0246 (9)0.0042 (8)0.0129 (8)0.0023 (8)
N3_60.0232 (11)0.0156 (11)0.0180 (10)0.0015 (9)0.0072 (9)0.0023 (9)
O8_60.0387 (11)0.0215 (10)0.0508 (12)0.0070 (9)0.0129 (9)0.0107 (9)
O9_60.0259 (9)0.0271 (10)0.0200 (8)0.0044 (8)0.0049 (7)0.0030 (7)
O10_60.0264 (9)0.0283 (10)0.0230 (9)0.0057 (8)0.0030 (7)0.0049 (8)
N4_70.0191 (11)0.0163 (11)0.0182 (10)0.0026 (9)0.0044 (9)0.0005 (9)
O8_70.0525 (12)0.0173 (10)0.0490 (12)0.0048 (9)0.0287 (10)0.0076 (9)
O9_70.0271 (10)0.0365 (11)0.0218 (9)0.0081 (8)0.0050 (8)0.0053 (8)
O10_70.0275 (9)0.0307 (10)0.0208 (9)0.0072 (8)0.0073 (7)0.0009 (8)
N5_80.0178 (11)0.0155 (11)0.0165 (10)0.0000 (9)0.0038 (9)0.0031 (8)
O8_80.0306 (10)0.0170 (9)0.0188 (8)0.0055 (7)0.0030 (7)0.0040 (7)
O9_80.0322 (10)0.0183 (9)0.0203 (8)0.0100 (8)0.0023 (7)0.0016 (7)
O10_80.0275 (9)0.0260 (10)0.0271 (9)0.0038 (8)0.0117 (8)0.0029 (8)
N6_90.0211 (11)0.0167 (11)0.0160 (10)0.0031 (9)0.0040 (9)0.0017 (9)
O8_90.0318 (10)0.0193 (9)0.0242 (9)0.0080 (8)0.0027 (8)0.0031 (7)
O9_90.0211 (9)0.0188 (9)0.0231 (9)0.0055 (7)0.0031 (7)0.0019 (7)
O10_90.0218 (9)0.0300 (10)0.0223 (9)0.0058 (8)0.0054 (7)0.0011 (8)
Geometric parameters (Å, º) top
Ni1_1—O6_11.989 (4)C4_2—H4A_20.9900
Ni1_1—O7_12.011 (4)C4_2—H4B_20.9900
Ni1_1—O3_12.050 (3)C5_2—C6_21.497 (3)
Ni1_1—O4_12.141 (3)C5_2—H5A_20.9900
Ni1_1—O5_12.142 (4)C5_2—H5B_20.9900
Ni1_1—O2_12.318 (3)C6_2—H6A_20.9900
Ni1_1—O1_12.508 (3)C6_2—H6B_20.9900
Ni1'_1—O7_11.971 (2)C7_2—C8_21.510 (3)
Ni1'_1—O6_11.999 (2)C7_2—H7A_20.9900
Ni1'_1—O2_12.055 (3)C7_2—H7B_20.9900
Ni1'_1—O1_12.119 (3)C8_2—H8A_20.9900
Ni1'_1—O5_12.160 (2)C8_2—H8B_20.9900
Ni1'_1—O3_12.290 (3)C9_2—C10_21.502 (3)
Ni1'_1—O4_12.537 (3)C9_2—H9A_20.9900
O1_1—C1_11.436 (2)C9_2—H9B_20.9900
O1_1—C10_11.444 (2)C10_2—H10A_20.9900
O2_1—C2_11.438 (2)C10_2—H10B_20.9900
O2_1—C3_11.440 (2)Ni3_3—O7_31.989 (4)
O3_1—C4_11.441 (2)Ni3_3—O6_31.990 (4)
O3_1—C5_11.449 (2)Ni3_3—O3_32.052 (4)
O4_1—C7_11.434 (2)Ni3_3—O5_32.141 (4)
O4_1—C6_11.439 (2)Ni3_3—O4_32.149 (3)
O5_1—C8_11.431 (2)Ni3_3—O2_32.302 (3)
O5_1—C9_11.434 (2)Ni3_3—O1_32.515 (3)
O6_1—H6W1_10.831 (9)Ni3'_3—O7_31.978 (3)
O6_1—H6W2_10.812 (9)Ni3'_3—O6_31.983 (3)
O7_1—H7W1_10.830 (9)Ni3'_3—O2_32.025 (3)
O7_1—H7W2_10.844 (9)Ni3'_3—O1_32.142 (3)
C1_1—C2_11.502 (3)Ni3'_3—O5_32.180 (3)
C1_1—H1A_10.9900Ni3'_3—O3_32.269 (3)
C1_1—H1B_10.9900Ni3'_3—O4_32.548 (3)
C2_1—H2A_10.9900O1_3—C10_31.437 (2)
C2_1—H2B_10.9900O1_3—C1_31.439 (2)
C3_1—C4_11.504 (3)O2_3—C3_31.438 (2)
C3_1—H3A_10.9900O2_3—C2_31.446 (2)
C3_1—H3B_10.9900O3_3—C4_31.431 (2)
C4_1—H4A_10.9900O3_3—C5_31.438 (2)
C4_1—H4B_10.9900O4_3—C7_31.432 (2)
C5_1—C6_11.503 (3)O4_3—C6_31.441 (2)
C5_1—H5A_10.9900O5_3—C8_31.431 (2)
C5_1—H5B_10.9900O5_3—C9_31.431 (2)
C6_1—H6A_10.9900O6_3—H6W1_30.831 (9)
C6_1—H6B_10.9900O6_3—H6W2_30.828 (9)
C7_1—C8_11.506 (3)O7_3—H7W1_30.828 (9)
C7_1—H7A_10.9900O7_3—H7W2_30.827 (9)
C7_1—H7B_10.9900C1_3—C2_31.506 (3)
C8_1—H8A_10.9900C1_3—H1A_30.9900
C8_1—H8B_10.9900C1_3—H1B_30.9900
C9_1—C10_11.507 (3)C2_3—H2A_30.9900
C9_1—H9A_10.9900C2_3—H2B_30.9900
C9_1—H9B_10.9900C3_3—C4_31.506 (3)
C10_1—H10A_10.9900C3_3—H3A_30.9900
C10_1—H10B_10.9900C3_3—H3B_30.9900
Ni2_2—O6_21.993 (3)C4_3—H4A_30.9900
Ni2_2—O7_21.995 (3)C4_3—H4B_30.9900
Ni2_2—O3_22.085 (4)C5_3—C6_31.497 (3)
Ni2_2—O4_22.119 (3)C5_3—H5A_30.9900
Ni2_2—O5_22.127 (4)C5_3—H5B_30.9900
Ni2_2—O2_22.334 (3)C6_3—H6A_30.9900
Ni2_2—O1_22.494 (3)C6_3—H6B_30.9900
Ni2'_2—O7_21.980 (3)C7_3—C8_31.505 (3)
Ni2'_2—O6_22.002 (3)C7_3—H7A_30.9900
Ni2'_2—O2_22.069 (3)C7_3—H7B_30.9900
Ni2'_2—O1_22.101 (3)C8_3—H8A_30.9900
Ni2'_2—O5_22.152 (3)C8_3—H8B_30.9900
Ni2'_2—O3_22.317 (3)C9_3—C10_31.502 (3)
Ni2'_2—O4_22.524 (3)C9_3—H9A_30.9900
O1_2—C10_21.437 (2)C9_3—H9B_30.9900
O1_2—C1_21.441 (2)C10_3—H10A_30.9900
O2_2—C2_21.431 (2)C10_3—H10B_30.9900
O2_2—C3_21.436 (2)N1_4—O10_41.235 (2)
O3_2—C4_21.439 (2)N1_4—O8_41.262 (2)
O3_2—C5_21.440 (2)N1_4—O9_41.266 (2)
O4_2—C7_21.428 (2)N2_5—O10_51.231 (2)
O4_2—C6_21.438 (2)N2_5—O9_51.261 (2)
O5_2—C9_21.431 (2)N2_5—O8_51.267 (2)
O5_2—C8_21.433 (2)N3_6—O10_61.238 (2)
O6_2—H6W1_20.829 (9)N3_6—O8_61.242 (2)
O6_2—H6W2_20.828 (9)N3_6—O9_61.273 (2)
O7_2—H7W1_20.835 (9)N4_7—O10_71.236 (2)
O7_2—H7W2_20.831 (9)N4_7—O8_71.243 (2)
C1_2—C2_21.502 (3)N4_7—O9_71.264 (2)
C1_2—H1A_20.9900N5_8—O10_81.236 (2)
C1_2—H1B_20.9900N5_8—O8_81.260 (2)
C2_2—H2A_20.9900N5_8—O9_81.263 (2)
C2_2—H2B_20.9900N6_9—O10_91.237 (2)
C3_2—C4_21.501 (3)N6_9—O9_91.263 (2)
C3_2—H3A_20.9900N6_9—O8_91.264 (2)
C3_2—H3B_20.9900
O6_1—Ni1_1—O7_1163.42 (18)O1_2—C1_2—H1A_2110.5
O6_1—Ni1_1—O3_190.37 (14)C2_2—C1_2—H1A_2110.5
O7_1—Ni1_1—O3_1100.42 (16)O1_2—C1_2—H1B_2110.5
O6_1—Ni1_1—O4_1100.79 (16)C2_2—C1_2—H1B_2110.5
O7_1—Ni1_1—O4_193.50 (14)H1A_2—C1_2—H1B_2108.7
O3_1—Ni1_1—O4_180.13 (12)O2_2—C2_2—C1_2106.06 (17)
O6_1—Ni1_1—O5_187.17 (14)O2_2—C2_2—H2A_2110.5
O7_1—Ni1_1—O5_188.86 (14)C1_2—C2_2—H2A_2110.5
O3_1—Ni1_1—O5_1152.60 (17)O2_2—C2_2—H2B_2110.5
O4_1—Ni1_1—O5_173.57 (12)C1_2—C2_2—H2B_2110.5
O6_1—Ni1_1—O2_192.58 (14)H2A_2—C2_2—H2B_2108.7
O7_1—Ni1_1—O2_178.56 (13)O2_2—C3_2—C4_2105.52 (17)
O3_1—Ni1_1—O2_173.92 (12)O2_2—C3_2—H3A_2110.6
O4_1—Ni1_1—O2_1150.83 (17)C4_2—C3_2—H3A_2110.6
O5_1—Ni1_1—O2_1133.43 (15)O2_2—C3_2—H3B_2110.6
O6_1—Ni1_1—O1_182.10 (12)C4_2—C3_2—H3B_2110.6
O7_1—Ni1_1—O1_181.53 (12)H3A_2—C3_2—H3B_2108.8
O3_1—Ni1_1—O1_1139.60 (16)O3_2—C4_2—C3_2106.45 (17)
O4_1—Ni1_1—O1_1140.26 (16)O3_2—C4_2—H4A_2110.4
O5_1—Ni1_1—O1_166.96 (10)C3_2—C4_2—H4A_2110.4
O2_1—Ni1_1—O1_166.90 (9)O3_2—C4_2—H4B_2110.4
O7_1—Ni1'_1—O6_1171.59 (18)C3_2—C4_2—H4B_2110.4
O7_1—Ni1'_1—O2_186.21 (9)H4A_2—C4_2—H4B_2108.6
O6_1—Ni1'_1—O2_1100.74 (10)O3_2—C5_2—C6_2106.24 (17)
O7_1—Ni1'_1—O1_193.28 (11)O3_2—C5_2—H5A_2110.5
O6_1—Ni1'_1—O1_192.66 (11)C6_2—C5_2—H5A_2110.5
O2_1—Ni1'_1—O1_179.36 (12)O3_2—C5_2—H5B_2110.5
O7_1—Ni1'_1—O5_189.43 (8)C6_2—C5_2—H5B_2110.5
O6_1—Ni1'_1—O5_186.46 (8)H5A_2—C5_2—H5B_2108.7
O2_1—Ni1'_1—O5_1152.99 (16)O4_2—C6_2—C5_2106.40 (17)
O1_1—Ni1'_1—O5_174.29 (8)O4_2—C6_2—H6A_2110.4
O7_1—Ni1'_1—O3_193.88 (10)C5_2—C6_2—H6A_2110.4
O6_1—Ni1'_1—O3_183.56 (9)O4_2—C6_2—H6B_2110.4
O2_1—Ni1'_1—O3_174.46 (7)C5_2—C6_2—H6B_2110.4
O1_1—Ni1'_1—O3_1152.30 (12)H6A_2—C6_2—H6B_2108.6
O5_1—Ni1'_1—O3_1132.48 (15)O4_2—C7_2—C8_2106.19 (17)
O7_1—Ni1'_1—O4_183.30 (10)O4_2—C7_2—H7A_2110.5
O6_1—Ni1'_1—O4_188.32 (11)C8_2—C7_2—H7A_2110.5
O2_1—Ni1'_1—O4_1139.83 (12)O4_2—C7_2—H7B_2110.5
O1_1—Ni1'_1—O4_1139.76 (8)C8_2—C7_2—H7B_2110.5
O5_1—Ni1'_1—O4_165.62 (8)H7A_2—C7_2—H7B_2108.7
O3_1—Ni1'_1—O4_167.75 (9)O5_2—C8_2—C7_2106.94 (17)
C1_1—O1_1—C10_1113.77 (15)O5_2—C8_2—H8A_2110.3
C1_1—O1_1—Ni1'_1108.67 (12)C7_2—C8_2—H8A_2110.3
C10_1—O1_1—Ni1'_1111.07 (12)O5_2—C8_2—H8B_2110.3
C1_1—O1_1—Ni1_1112.42 (14)C7_2—C8_2—H8B_2110.3
C10_1—O1_1—Ni1_1108.03 (13)H8A_2—C8_2—H8B_2108.6
C2_1—O2_1—C3_1114.65 (15)O5_2—C9_2—C10_2106.50 (17)
C2_1—O2_1—Ni1'_1111.19 (14)O5_2—C9_2—H9A_2110.4
C3_1—O2_1—Ni1'_1115.91 (14)C10_2—C9_2—H9A_2110.4
C2_1—O2_1—Ni1_1119.38 (14)O5_2—C9_2—H9B_2110.4
C3_1—O2_1—Ni1_1108.42 (14)C10_2—C9_2—H9B_2110.4
C4_1—O3_1—C5_1113.87 (15)H9A_2—C9_2—H9B_2108.6
C4_1—O3_1—Ni1_1118.21 (15)O1_2—C10_2—C9_2105.79 (17)
C5_1—O3_1—Ni1_1108.80 (14)O1_2—C10_2—H10A_2110.6
C4_1—O3_1—Ni1'_1109.73 (13)C9_2—C10_2—H10A_2110.6
C5_1—O3_1—Ni1'_1116.95 (13)O1_2—C10_2—H10B_2110.6
C7_1—O4_1—C6_1114.06 (16)C9_2—C10_2—H10B_2110.6
C7_1—O4_1—Ni1_1109.48 (15)H10A_2—C10_2—H10B_2108.7
C6_1—O4_1—Ni1_1108.06 (15)O7_3—Ni3_3—O6_3165.41 (17)
C7_1—O4_1—Ni1'_1107.55 (12)O7_3—Ni3_3—O3_3100.25 (16)
C6_1—O4_1—Ni1'_1111.45 (12)O6_3—Ni3_3—O3_388.35 (15)
C8_1—O5_1—C9_1114.90 (15)O7_3—Ni3_3—O5_388.07 (15)
C8_1—O5_1—Ni1_1117.95 (14)O6_3—Ni3_3—O5_389.62 (15)
C9_1—O5_1—Ni1_1127.12 (14)O3_3—Ni3_3—O5_3152.54 (15)
C8_1—O5_1—Ni1'_1129.13 (14)O7_3—Ni3_3—O4_393.61 (14)
C9_1—O5_1—Ni1'_1115.95 (14)O6_3—Ni3_3—O4_399.60 (15)
Ni1_1—O6_1—H6W1_1121.5 (15)O3_3—Ni3_3—O4_379.26 (12)
Ni1'_1—O6_1—H6W1_1118.7 (15)O5_3—Ni3_3—O4_374.10 (11)
Ni1_1—O6_1—H6W2_1130.1 (15)O7_3—Ni3_3—O2_380.00 (12)
Ni1'_1—O6_1—H6W2_1130.5 (15)O6_3—Ni3_3—O2_391.19 (13)
H6W1_1—O6_1—H6W2_1108.3 (14)O3_3—Ni3_3—O2_374.18 (12)
Ni1'_1—O7_1—H7W1_1130.7 (15)O5_3—Ni3_3—O2_3133.25 (15)
Ni1_1—O7_1—H7W1_1127.8 (15)O4_3—Ni3_3—O2_3150.98 (18)
Ni1'_1—O7_1—H7W2_1118.1 (15)O7_3—Ni3_3—O1_385.00 (13)
Ni1_1—O7_1—H7W2_1113.3 (15)O6_3—Ni3_3—O1_380.84 (12)
H7W1_1—O7_1—H7W2_1105.8 (13)O3_3—Ni3_3—O1_3139.40 (14)
O1_1—C1_1—C2_1106.28 (17)O5_3—Ni3_3—O1_366.92 (11)
O1_1—C1_1—H1A_1110.5O4_3—Ni3_3—O1_3141.01 (17)
C2_1—C1_1—H1A_1110.5O2_3—Ni3_3—O1_367.12 (8)
O1_1—C1_1—H1B_1110.5O7_3—Ni3'_3—O6_3170.26 (17)
C2_1—C1_1—H1B_1110.5O7_3—Ni3'_3—O2_387.54 (11)
H1A_1—C1_1—H1B_1108.7O6_3—Ni3'_3—O2_3100.15 (12)
O2_1—C2_1—C1_1105.91 (17)O7_3—Ni3'_3—O1_396.17 (11)
O2_1—C2_1—H2A_1110.6O6_3—Ni3'_3—O1_391.13 (11)
C1_1—C2_1—H2A_1110.6O2_3—Ni3'_3—O1_379.60 (11)
O2_1—C2_1—H2B_1110.6O7_3—Ni3'_3—O5_387.26 (10)
C1_1—C2_1—H2B_1110.6O6_3—Ni3'_3—O5_388.66 (10)
H2A_1—C2_1—H2B_1108.7O2_3—Ni3'_3—O5_3151.83 (14)
O2_1—C3_1—C4_1105.06 (16)O1_3—Ni3'_3—O5_373.48 (9)
O2_1—C3_1—H3A_1110.7O7_3—Ni3'_3—O3_393.59 (11)
C4_1—C3_1—H3A_1110.7O6_3—Ni3'_3—O3_382.69 (10)
O2_1—C3_1—H3B_1110.7O2_3—Ni3'_3—O3_375.42 (9)
C4_1—C3_1—H3B_1110.7O1_3—Ni3'_3—O3_3152.71 (13)
H3A_1—C3_1—H3B_1108.8O5_3—Ni3'_3—O3_3132.55 (13)
O3_1—C4_1—C3_1105.85 (16)O7_3—Ni3'_3—O4_382.65 (11)
O3_1—C4_1—H4A_1110.6O6_3—Ni3'_3—O4_387.61 (11)
C3_1—C4_1—H4A_1110.6O2_3—Ni3'_3—O4_3140.65 (12)
O3_1—C4_1—H4B_1110.6O1_3—Ni3'_3—O4_3139.21 (11)
C3_1—C4_1—H4B_1110.6O5_3—Ni3'_3—O4_365.74 (8)
H4A_1—C4_1—H4B_1108.7O3_3—Ni3'_3—O4_367.35 (8)
O3_1—C5_1—C6_1106.10 (17)C10_3—O1_3—C1_3113.49 (16)
O3_1—C5_1—H5A_1110.5C10_3—O1_3—Ni3'_3112.18 (13)
C6_1—C5_1—H5A_1110.5C1_3—O1_3—Ni3'_3107.91 (13)
O3_1—C5_1—H5B_1110.5C10_3—O1_3—Ni3_3108.64 (14)
C6_1—C5_1—H5B_1110.5C1_3—O1_3—Ni3_3112.06 (14)
H5A_1—C5_1—H5B_1108.7C3_3—O2_3—C2_3113.89 (15)
O4_1—C6_1—C5_1106.02 (17)C3_3—O2_3—Ni3'_3116.15 (14)
O4_1—C6_1—H6A_1110.5C2_3—O2_3—Ni3'_3111.98 (14)
C5_1—C6_1—H6A_1110.5C3_3—O2_3—Ni3_3109.16 (15)
O4_1—C6_1—H6B_1110.5C2_3—O2_3—Ni3_3119.79 (14)
C5_1—C6_1—H6B_1110.5C4_3—O3_3—C5_3114.28 (16)
H6A_1—C6_1—H6B_1108.7C4_3—O3_3—Ni3_3117.29 (14)
O4_1—C7_1—C8_1106.28 (17)C5_3—O3_3—Ni3_3110.74 (14)
O4_1—C7_1—H7A_1110.5C4_3—O3_3—Ni3'_3108.92 (13)
C8_1—C7_1—H7A_1110.5C5_3—O3_3—Ni3'_3119.53 (14)
O4_1—C7_1—H7B_1110.5C7_3—O4_3—C6_3113.94 (16)
C8_1—C7_1—H7B_1110.5C7_3—O4_3—Ni3_3109.29 (15)
H7A_1—C7_1—H7B_1108.7C6_3—O4_3—Ni3_3108.08 (15)
O5_1—C8_1—C7_1106.28 (16)C7_3—O4_3—Ni3'_3107.46 (13)
O5_1—C8_1—H8A_1110.5C6_3—O4_3—Ni3'_3110.63 (13)
C7_1—C8_1—H8A_1110.5C8_3—O5_3—C9_3115.37 (15)
O5_1—C8_1—H8B_1110.5C8_3—O5_3—Ni3_3117.23 (14)
C7_1—C8_1—H8B_1110.5C9_3—O5_3—Ni3_3126.98 (14)
H8A_1—C8_1—H8B_1108.7C8_3—O5_3—Ni3'_3128.13 (14)
O5_1—C9_1—C10_1106.66 (16)C9_3—O5_3—Ni3'_3116.11 (13)
O5_1—C9_1—H9A_1110.4Ni3'_3—O6_3—H6W1_3121.3 (14)
C10_1—C9_1—H9A_1110.4Ni3_3—O6_3—H6W1_3122.1 (14)
O5_1—C9_1—H9B_1110.4Ni3'_3—O6_3—H6W2_3131.2 (14)
C10_1—C9_1—H9B_1110.4Ni3_3—O6_3—H6W2_3126.5 (15)
H9A_1—C9_1—H9B_1108.6H6W1_3—O6_3—H6W2_3106.8 (13)
O1_1—C10_1—C9_1104.77 (16)Ni3'_3—O7_3—H7W1_3128.7 (15)
O1_1—C10_1—H10A_1110.8Ni3_3—O7_3—H7W1_3128.3 (16)
C9_1—C10_1—H10A_1110.8Ni3'_3—O7_3—H7W2_3120.8 (15)
O1_1—C10_1—H10B_1110.8Ni3_3—O7_3—H7W2_3115.8 (16)
C9_1—C10_1—H10B_1110.8H7W1_3—O7_3—H7W2_3108.3 (14)
H10A_1—C10_1—H10B_1108.9O1_3—C1_3—C2_3106.33 (18)
O6_2—Ni2_2—O7_2166.58 (16)O1_3—C1_3—H1A_3110.5
O6_2—Ni2_2—O3_288.44 (14)C2_3—C1_3—H1A_3110.5
O7_2—Ni2_2—O3_2100.37 (15)O1_3—C1_3—H1B_3110.5
O6_2—Ni2_2—O4_297.27 (13)C2_3—C1_3—H1B_3110.5
O7_2—Ni2_2—O4_294.26 (13)H1A_3—C1_3—H1B_3108.7
O3_2—Ni2_2—O4_279.87 (11)O2_3—C2_3—C1_3105.71 (17)
O6_2—Ni2_2—O5_288.26 (14)O2_3—C2_3—H2A_3110.6
O7_2—Ni2_2—O5_288.28 (14)C1_3—C2_3—H2A_3110.6
O3_2—Ni2_2—O5_2153.25 (14)O2_3—C2_3—H2B_3110.6
O4_2—Ni2_2—O5_274.24 (11)C1_3—C2_3—H2B_3110.6
O6_2—Ni2_2—O2_294.23 (12)H2A_3—C2_3—H2B_3108.7
O7_2—Ni2_2—O2_278.97 (11)O2_3—C3_3—C4_3105.10 (16)
O3_2—Ni2_2—O2_272.69 (11)O2_3—C3_3—H3A_3110.7
O4_2—Ni2_2—O2_2149.87 (17)C4_3—C3_3—H3A_3110.7
O5_2—Ni2_2—O2_2134.04 (14)O2_3—C3_3—H3B_3110.7
O6_2—Ni2_2—O1_282.99 (11)C4_3—C3_3—H3B_3110.7
O7_2—Ni2_2—O1_283.69 (11)H3A_3—C3_3—H3B_3108.8
O3_2—Ni2_2—O1_2137.78 (14)O3_3—C4_3—C3_3106.01 (17)
O4_2—Ni2_2—O1_2142.16 (17)O3_3—C4_3—H4A_3110.5
O5_2—Ni2_2—O1_267.94 (10)C3_3—C4_3—H4A_3110.5
O2_2—Ni2_2—O1_266.87 (8)O3_3—C4_3—H4B_3110.5
O7_2—Ni2'_2—O6_2168.35 (16)C3_3—C4_3—H4B_3110.5
O7_2—Ni2'_2—O2_286.13 (11)H4A_3—C4_3—H4B_3108.7
O6_2—Ni2'_2—O2_2102.66 (12)O3_3—C5_3—C6_3106.25 (18)
O7_2—Ni2'_2—O1_295.35 (11)O3_3—C5_3—H5A_3110.5
O6_2—Ni2'_2—O1_293.80 (12)C6_3—C5_3—H5A_3110.5
O2_2—Ni2'_2—O1_279.40 (10)O3_3—C5_3—H5B_3110.5
O7_2—Ni2'_2—O5_288.00 (11)C6_3—C5_3—H5B_3110.5
O6_2—Ni2'_2—O5_287.35 (11)H5A_3—C5_3—H5B_3108.7
O2_2—Ni2'_2—O5_2153.42 (14)O4_3—C6_3—C5_3106.27 (18)
O1_2—Ni2'_2—O5_275.37 (10)O4_3—C6_3—H6A_3110.5
O7_2—Ni2'_2—O3_293.38 (11)C5_3—C6_3—H6A_3110.5
O6_2—Ni2'_2—O3_282.05 (10)O4_3—C6_3—H6B_3110.5
O2_2—Ni2'_2—O3_273.33 (9)C5_3—C6_3—H6B_3110.5
O1_2—Ni2'_2—O3_2150.68 (14)H6A_3—C6_3—H6B_3108.7
O5_2—Ni2'_2—O3_2132.96 (13)O4_3—C7_3—C8_3106.37 (17)
O7_2—Ni2'_2—O4_283.16 (10)O4_3—C7_3—H7A_3110.5
O6_2—Ni2'_2—O4_285.18 (10)C8_3—C7_3—H7A_3110.5
O2_2—Ni2'_2—O4_2138.65 (12)O4_3—C7_3—H7B_3110.5
O1_2—Ni2'_2—O4_2141.26 (13)C8_3—C7_3—H7B_3110.5
O5_2—Ni2'_2—O4_265.90 (9)H7A_3—C7_3—H7B_3108.6
O3_2—Ni2'_2—O4_267.61 (8)O5_3—C8_3—C7_3106.99 (17)
C10_2—O1_2—C1_2112.98 (16)O5_3—C8_3—H8A_3110.3
C10_2—O1_2—Ni2'_2110.98 (14)C7_3—C8_3—H8A_3110.3
C1_2—O1_2—Ni2'_2108.80 (14)O5_3—C8_3—H8B_3110.3
C10_2—O1_2—Ni2_2107.73 (14)C7_3—C8_3—H8B_3110.3
C1_2—O1_2—Ni2_2112.46 (14)H8A_3—C8_3—H8B_3108.6
C2_2—O2_2—C3_2114.27 (15)O5_3—C9_3—C10_3106.89 (16)
C2_2—O2_2—Ni2'_2111.15 (14)O5_3—C9_3—H9A_3110.3
C3_2—O2_2—Ni2'_2117.82 (14)C10_3—C9_3—H9A_3110.3
C2_2—O2_2—Ni2_2119.51 (14)O5_3—C9_3—H9B_3110.3
C3_2—O2_2—Ni2_2110.44 (14)C10_3—C9_3—H9B_3110.3
C4_2—O3_2—C5_2113.78 (15)H9A_3—C9_3—H9B_3108.6
C4_2—O3_2—Ni2_2118.54 (14)O1_3—C10_3—C9_3104.99 (16)
C5_2—O3_2—Ni2_2108.12 (14)O1_3—C10_3—H10A_3110.7
C4_2—O3_2—Ni2'_2110.26 (13)C9_3—C10_3—H10A_3110.7
C5_2—O3_2—Ni2'_2116.68 (13)O1_3—C10_3—H10B_3110.7
C7_2—O4_2—C6_2114.03 (16)C9_3—C10_3—H10B_3110.7
C7_2—O4_2—Ni2_2110.10 (15)H10A_3—C10_3—H10B_3108.8
C6_2—O4_2—Ni2_2108.74 (15)O10_4—N1_4—O8_4121.15 (19)
C7_2—O4_2—Ni2'_2107.94 (13)O10_4—N1_4—O9_4120.25 (19)
C6_2—O4_2—Ni2'_2111.73 (13)O8_4—N1_4—O9_4118.58 (17)
C9_2—O5_2—C8_2115.77 (15)O10_5—N2_5—O9_5121.13 (19)
C9_2—O5_2—Ni2_2126.29 (13)O10_5—N2_5—O8_5120.69 (19)
C8_2—O5_2—Ni2_2117.38 (14)O9_5—N2_5—O8_5118.17 (17)
C9_2—O5_2—Ni2'_2114.99 (13)O10_6—N3_6—O8_6121.59 (19)
C8_2—O5_2—Ni2'_2128.67 (14)O10_6—N3_6—O9_6119.32 (18)
Ni2_2—O6_2—H6W1_2120.2 (15)O8_6—N3_6—O9_6119.08 (19)
Ni2'_2—O6_2—H6W1_2116.9 (16)O10_7—N4_7—O8_7121.52 (19)
Ni2_2—O6_2—H6W2_2123.8 (15)O10_7—N4_7—O9_7119.68 (19)
Ni2'_2—O6_2—H6W2_2118.1 (16)O8_7—N4_7—O9_7118.78 (19)
H6W1_2—O6_2—H6W2_2107.0 (14)O10_8—N5_8—O8_8120.97 (18)
Ni2'_2—O7_2—H7W1_2121.7 (15)O10_8—N5_8—O9_8120.34 (18)
Ni2_2—O7_2—H7W1_2114.8 (15)O8_8—N5_8—O9_8118.67 (17)
Ni2'_2—O7_2—H7W2_2126.6 (15)O10_9—N6_9—O9_9120.56 (18)
Ni2_2—O7_2—H7W2_2125.7 (15)O10_9—N6_9—O8_9120.96 (19)
H7W1_2—O7_2—H7W2_2105.6 (13)O9_9—N6_9—O8_9118.47 (18)
O1_2—C1_2—C2_2106.27 (17)
O7_1—Ni1'_1—O1_1—C1_168.66 (14)O6_2—Ni2_2—O4_2—Ni2'_296 (3)
O6_1—Ni1'_1—O1_1—C1_1117.30 (14)O7_2—Ni2_2—O4_2—Ni2'_277 (3)
O2_1—Ni1'_1—O1_1—C1_116.86 (13)O3_2—Ni2_2—O4_2—Ni2'_2176 (3)
O5_1—Ni1'_1—O1_1—C1_1157.14 (13)O5_2—Ni2_2—O4_2—Ni2'_210 (3)
O3_1—Ni1'_1—O1_1—C1_136.1 (3)O2_2—Ni2_2—O4_2—Ni2'_2152 (3)
O4_1—Ni1'_1—O1_1—C1_1152.16 (14)O1_2—Ni2_2—O4_2—Ni2'_29 (2)
O7_1—Ni1'_1—O1_1—C10_157.23 (15)O7_2—Ni2'_2—O4_2—C7_2124.27 (14)
O6_1—Ni1'_1—O1_1—C10_1116.82 (14)O6_2—Ni2'_2—O4_2—C7_255.84 (14)
O2_1—Ni1'_1—O1_1—C10_1142.75 (13)O2_2—Ni2'_2—O4_2—C7_2159.56 (18)
O5_1—Ni1'_1—O1_1—C10_131.25 (13)O1_2—Ni2'_2—O4_2—C7_234.2 (2)
O3_1—Ni1'_1—O1_1—C10_1161.99 (19)O5_2—Ni2'_2—O4_2—C7_233.40 (13)
O4_1—Ni1'_1—O1_1—C10_126.3 (2)O3_2—Ni2'_2—O4_2—C7_2139.21 (13)
O7_1—Ni1'_1—O1_1—Ni1_196.1 (17)O7_2—Ni2'_2—O4_2—C6_2109.59 (15)
O6_1—Ni1'_1—O1_1—Ni1_177.9 (17)O6_2—Ni2'_2—O4_2—C6_270.30 (15)
O2_1—Ni1'_1—O1_1—Ni1_1178.3 (17)O2_2—Ni2'_2—O4_2—C6_233.4 (2)
O5_1—Ni1'_1—O1_1—Ni1_17.7 (17)O1_2—Ni2'_2—O4_2—C6_2160.37 (19)
O3_1—Ni1'_1—O1_1—Ni1_1159.1 (19)O5_2—Ni2'_2—O4_2—C6_2159.54 (14)
O4_1—Ni1'_1—O1_1—Ni1_112.6 (16)O3_2—Ni2'_2—O4_2—C6_213.07 (14)
O6_1—Ni1_1—O1_1—C1_1113.39 (15)O7_2—Ni2'_2—O4_2—Ni2_2100 (3)
O7_1—Ni1_1—O1_1—C1_163.95 (16)O6_2—Ni2'_2—O4_2—Ni2_280 (3)
O3_1—Ni1_1—O1_1—C1_132.2 (3)O2_2—Ni2'_2—O4_2—Ni2_224 (2)
O4_1—Ni1_1—O1_1—C1_1149.2 (2)O1_2—Ni2'_2—O4_2—Ni2_2170 (3)
O5_1—Ni1_1—O1_1—C1_1156.33 (14)O5_2—Ni2'_2—O4_2—Ni2_2169 (3)
O2_1—Ni1_1—O1_1—C1_117.16 (15)O3_2—Ni2'_2—O4_2—Ni2_23 (3)
O6_1—Ni1_1—O1_1—C10_1120.25 (15)O6_2—Ni2_2—O5_2—C9_280.67 (19)
O7_1—Ni1_1—O1_1—C10_162.41 (16)O7_2—Ni2_2—O5_2—C9_286.36 (19)
O3_1—Ni1_1—O1_1—C10_1158.6 (2)O3_2—Ni2_2—O5_2—C9_2163.7 (3)
O4_1—Ni1_1—O1_1—C10_122.9 (3)O4_2—Ni2_2—O5_2—C9_2178.72 (16)
O5_1—Ni1_1—O1_1—C10_129.97 (15)O2_2—Ni2_2—O5_2—C9_213.5 (3)
O2_1—Ni1_1—O1_1—C10_1143.52 (14)O1_2—Ni2_2—O5_2—C9_22.47 (18)
O6_1—Ni1_1—O1_1—Ni1'_197.8 (17)O6_2—Ni2_2—O5_2—C8_290.31 (16)
O7_1—Ni1_1—O1_1—Ni1'_179.5 (17)O7_2—Ni2_2—O5_2—C8_2102.66 (16)
O3_1—Ni1_1—O1_1—Ni1'_116.6 (15)O3_2—Ni2_2—O5_2—C8_27.2 (4)
O4_1—Ni1_1—O1_1—Ni1'_1164.8 (19)O4_2—Ni2_2—O5_2—C8_27.74 (17)
O5_1—Ni1_1—O1_1—Ni1'_1171.9 (18)O2_2—Ni2_2—O5_2—C8_2175.49 (19)
O2_1—Ni1_1—O1_1—Ni1'_11.6 (17)O1_2—Ni2_2—O5_2—C8_2173.45 (15)
O7_1—Ni1'_1—O2_1—C2_1109.88 (15)O6_2—Ni2_2—O5_2—Ni2'_285.2 (7)
O6_1—Ni1'_1—O2_1—C2_174.89 (17)O7_2—Ni2_2—O5_2—Ni2'_281.8 (7)
O1_1—Ni1'_1—O2_1—C2_115.82 (13)O3_2—Ni2_2—O5_2—Ni2'_2168.3 (11)
O5_1—Ni1'_1—O2_1—C2_128.6 (3)O4_2—Ni2_2—O5_2—Ni2'_2176.7 (8)
O3_1—Ni1'_1—O2_1—C2_1155.03 (14)O2_2—Ni2_2—O5_2—Ni2'_29.0 (5)
O4_1—Ni1'_1—O2_1—C2_1175.18 (14)O1_2—Ni2_2—O5_2—Ni2'_22.1 (7)
O7_1—Ni1'_1—O2_1—C3_1116.83 (15)O7_2—Ni2'_2—O5_2—C9_297.74 (16)
O6_1—Ni1'_1—O2_1—C3_158.40 (18)O6_2—Ni2'_2—O5_2—C9_292.94 (15)
O1_1—Ni1'_1—O2_1—C3_1149.11 (14)O2_2—Ni2'_2—O5_2—C9_220.5 (4)
O5_1—Ni1'_1—O2_1—C3_1161.9 (2)O1_2—Ni2'_2—O5_2—C9_21.68 (15)
O3_1—Ni1'_1—O2_1—C3_121.74 (14)O3_2—Ni2'_2—O5_2—C9_2169.50 (16)
O4_1—Ni1'_1—O2_1—C3_141.9 (2)O4_2—Ni2'_2—O5_2—C9_2178.85 (14)
O7_1—Ni1'_1—O2_1—Ni1_186.8 (8)O7_2—Ni2'_2—O5_2—C8_291.39 (18)
O6_1—Ni1'_1—O2_1—Ni1_188.5 (8)O6_2—Ni2'_2—O5_2—C8_277.92 (19)
O1_1—Ni1'_1—O2_1—Ni1_1179.2 (9)O2_2—Ni2'_2—O5_2—C8_2168.6 (3)
O5_1—Ni1'_1—O2_1—Ni1_1168.0 (10)O1_2—Ni2'_2—O5_2—C8_2172.55 (17)
O3_1—Ni1'_1—O2_1—Ni1_18.3 (8)O3_2—Ni2'_2—O5_2—C8_21.4 (3)
O4_1—Ni1'_1—O2_1—Ni1_111.8 (7)O4_2—Ni2'_2—O5_2—C8_27.99 (17)
O6_1—Ni1_1—O2_1—C2_163.18 (18)O7_2—Ni2'_2—O5_2—Ni2_286.3 (7)
O7_1—Ni1_1—O2_1—C2_1102.68 (16)O6_2—Ni2'_2—O5_2—Ni2_283.0 (7)
O3_1—Ni1_1—O2_1—C2_1152.82 (15)O2_2—Ni2'_2—O5_2—Ni2_2163.5 (10)
O4_1—Ni1_1—O2_1—C2_1179.1 (3)O1_2—Ni2'_2—O5_2—Ni2_2177.6 (8)
O5_1—Ni1_1—O2_1—C2_125.4 (3)O3_2—Ni2'_2—O5_2—Ni2_26.5 (6)
O1_1—Ni1_1—O2_1—C2_117.10 (16)O4_2—Ni2'_2—O5_2—Ni2_22.9 (7)
O6_1—Ni1_1—O2_1—C3_170.62 (16)O7_2—Ni2_2—O6_2—Ni2'_212.6 (3)
O7_1—Ni1_1—O2_1—C3_1123.52 (15)O3_2—Ni2_2—O6_2—Ni2'_2118.7 (8)
O3_1—Ni1_1—O2_1—C3_119.02 (16)O4_2—Ni2_2—O6_2—Ni2'_2161.7 (9)
O4_1—Ni1_1—O2_1—C3_147.1 (4)O5_2—Ni2_2—O6_2—Ni2'_287.8 (8)
O5_1—Ni1_1—O2_1—C3_1159.2 (2)O2_2—Ni2_2—O6_2—Ni2'_246.2 (7)
O1_1—Ni1_1—O2_1—C3_1150.90 (13)O1_2—Ni2_2—O6_2—Ni2'_219.8 (7)
O6_1—Ni1_1—O2_1—Ni1'_181.0 (8)O7_2—Ni2'_2—O6_2—Ni2_214.7 (4)
O7_1—Ni1_1—O2_1—Ni1'_184.8 (8)O2_2—Ni2'_2—O6_2—Ni2_2123.6 (8)
O3_1—Ni1_1—O2_1—Ni1'_1170.7 (9)O1_2—Ni2'_2—O6_2—Ni2_2156.4 (9)
O4_1—Ni1_1—O2_1—Ni1'_1161.3 (11)O5_2—Ni2'_2—O6_2—Ni2_281.3 (8)
O5_1—Ni1_1—O2_1—Ni1'_17.5 (6)O3_2—Ni2'_2—O6_2—Ni2_252.8 (8)
O1_1—Ni1_1—O2_1—Ni1'_10.7 (8)O4_2—Ni2'_2—O6_2—Ni2_215.2 (7)
O6_1—Ni1_1—O3_1—C4_1107.00 (17)O6_2—Ni2'_2—O7_2—Ni2_214.6 (4)
O7_1—Ni1_1—O3_1—C4_160.34 (19)O2_2—Ni2'_2—O7_2—Ni2_2124.8 (8)
O4_1—Ni1_1—O3_1—C4_1152.12 (14)O1_2—Ni2'_2—O7_2—Ni2_2156.2 (9)
O5_1—Ni1_1—O3_1—C4_1168.5 (4)O5_2—Ni2'_2—O7_2—Ni2_281.1 (8)
O2_1—Ni1_1—O3_1—C4_114.42 (17)O3_2—Ni2'_2—O7_2—Ni2_251.8 (7)
O1_1—Ni1_1—O3_1—C4_128.8 (3)O4_2—Ni2'_2—O7_2—Ni2_215.1 (7)
O6_1—Ni1_1—O3_1—C5_1121.12 (16)O6_2—Ni2_2—O7_2—Ni2'_212.7 (3)
O7_1—Ni1_1—O3_1—C5_171.54 (18)O3_2—Ni2_2—O7_2—Ni2'_2117.6 (8)
O4_1—Ni1_1—O3_1—C5_120.24 (17)O4_2—Ni2_2—O7_2—Ni2'_2161.9 (9)
O5_1—Ni1_1—O3_1—C5_136.6 (4)O5_2—Ni2_2—O7_2—Ni2'_287.9 (8)
O2_1—Ni1_1—O3_1—C5_1146.30 (14)O2_2—Ni2_2—O7_2—Ni2'_247.7 (7)
O1_1—Ni1_1—O3_1—C5_1160.7 (2)O1_2—Ni2_2—O7_2—Ni2'_219.9 (7)
O6_1—Ni1_1—O3_1—Ni1'_184.7 (8)C10_2—O1_2—C1_2—C2_2169.30 (17)
O7_1—Ni1_1—O3_1—Ni1'_182.6 (8)Ni2'_2—O1_2—C1_2—C2_245.6 (2)
O4_1—Ni1_1—O3_1—Ni1'_1174.4 (9)Ni2_2—O1_2—C1_2—C2_247.1 (2)
O5_1—Ni1_1—O3_1—Ni1'_1169.2 (12)C3_2—O2_2—C2_2—C1_2179.09 (17)
O2_1—Ni1_1—O3_1—Ni1'_17.9 (8)Ni2'_2—O2_2—C2_2—C1_242.8 (2)
O1_1—Ni1_1—O3_1—Ni1'_16.5 (6)Ni2_2—O2_2—C2_2—C1_245.0 (2)
O7_1—Ni1'_1—O3_1—C4_173.04 (15)O1_2—C1_2—C2_2—O2_258.2 (2)
O6_1—Ni1'_1—O3_1—C4_1115.00 (14)C2_2—O2_2—C3_2—C4_2178.87 (17)
O2_1—Ni1'_1—O3_1—C4_111.93 (13)Ni2'_2—O2_2—C3_2—C4_247.9 (2)
O1_1—Ni1'_1—O3_1—C4_131.6 (3)Ni2_2—O2_2—C3_2—C4_243.0 (2)
O5_1—Ni1'_1—O3_1—C4_1165.82 (14)C5_2—O3_2—C4_2—C3_2173.36 (17)
O4_1—Ni1'_1—O3_1—C4_1154.18 (13)Ni2_2—O3_2—C4_2—C3_244.6 (2)
O7_1—Ni1'_1—O3_1—C5_158.60 (17)Ni2'_2—O3_2—C4_2—C3_240.06 (19)
O6_1—Ni1'_1—O3_1—C5_1113.36 (16)O2_2—C3_2—C4_2—O3_255.3 (2)
O2_1—Ni1'_1—O3_1—C5_1143.57 (15)C4_2—O3_2—C5_2—C6_2177.47 (16)
O1_1—Ni1'_1—O3_1—C5_1163.2 (2)Ni2_2—O3_2—C5_2—C6_248.6 (2)
O5_1—Ni1'_1—O3_1—C5_134.17 (19)Ni2'_2—O3_2—C5_2—C6_252.4 (2)
O4_1—Ni1'_1—O3_1—C5_122.53 (14)C7_2—O4_2—C6_2—C5_2165.64 (17)
O7_1—Ni1'_1—O3_1—Ni1_186.1 (8)Ni2_2—O4_2—C6_2—C5_242.4 (2)
O6_1—Ni1'_1—O3_1—Ni1_185.8 (8)Ni2'_2—O4_2—C6_2—C5_242.9 (2)
O2_1—Ni1'_1—O3_1—Ni1_1171.1 (9)O3_2—C5_2—C6_2—O4_261.0 (2)
O1_1—Ni1'_1—O3_1—Ni1_1169.2 (10)C6_2—O4_2—C7_2—C8_2177.41 (17)
O5_1—Ni1'_1—O3_1—Ni1_16.6 (7)Ni2_2—O4_2—C7_2—C8_254.9 (2)
O4_1—Ni1'_1—O3_1—Ni1_15.0 (8)Ni2'_2—O4_2—C7_2—C8_252.63 (18)
O6_1—Ni1_1—O4_1—C7_149.31 (19)C9_2—O5_2—C8_2—C7_2153.52 (17)
O7_1—Ni1_1—O4_1—C7_1122.23 (16)Ni2_2—O5_2—C8_2—C7_218.4 (2)
O3_1—Ni1_1—O4_1—C7_1137.79 (14)Ni2'_2—O5_2—C8_2—C7_217.3 (3)
O5_1—Ni1_1—O4_1—C7_134.46 (15)O4_2—C7_2—C8_2—O5_246.2 (2)
O2_1—Ni1_1—O4_1—C7_1165.1 (3)C8_2—O5_2—C9_2—C10_2158.43 (17)
O1_1—Ni1_1—O4_1—C7_141.3 (3)Ni2_2—O5_2—C9_2—C10_230.5 (2)
O6_1—Ni1_1—O4_1—C6_175.46 (18)Ni2'_2—O5_2—C9_2—C10_229.5 (2)
O7_1—Ni1_1—O4_1—C6_1113.00 (16)C1_2—O1_2—C10_2—C9_2175.56 (17)
O3_1—Ni1_1—O4_1—C6_113.02 (17)Ni2'_2—O1_2—C10_2—C9_253.1 (2)
O5_1—Ni1_1—O4_1—C6_1159.22 (15)Ni2_2—O1_2—C10_2—C9_250.7 (2)
O2_1—Ni1_1—O4_1—C6_140.3 (4)O5_2—C9_2—C10_2—O1_252.3 (2)
O1_1—Ni1_1—O4_1—C6_1166.0 (2)O7_3—Ni3'_3—O1_3—C10_355.95 (16)
O6_1—Ni1_1—O4_1—Ni1'_1105 (2)O6_3—Ni3'_3—O1_3—C10_3117.60 (15)
O7_1—Ni1_1—O4_1—Ni1'_166 (2)O2_3—Ni3'_3—O1_3—C10_3142.29 (14)
O3_1—Ni1_1—O4_1—Ni1'_1166 (2)O5_3—Ni3'_3—O1_3—C10_329.33 (14)
O5_1—Ni1_1—O4_1—Ni1'_121 (2)O3_3—Ni3'_3—O1_3—C10_3166.2 (2)
O2_1—Ni1_1—O4_1—Ni1'_1139 (2)O4_3—Ni3'_3—O1_3—C10_329.9 (2)
O1_1—Ni1_1—O4_1—Ni1'_114.5 (19)O7_3—Ni3'_3—O1_3—C1_369.79 (16)
O7_1—Ni1'_1—O4_1—C7_1124.94 (13)O6_3—Ni3'_3—O1_3—C1_3116.67 (14)
O6_1—Ni1'_1—O4_1—C7_154.35 (14)O2_3—Ni3'_3—O1_3—C1_316.56 (14)
O2_1—Ni1'_1—O4_1—C7_1159.09 (15)O5_3—Ni3'_3—O1_3—C1_3155.07 (14)
O1_1—Ni1'_1—O4_1—C7_137.79 (19)O3_3—Ni3'_3—O1_3—C1_340.5 (3)
O5_1—Ni1'_1—O4_1—C7_132.52 (12)O4_3—Ni3'_3—O1_3—C1_3155.67 (17)
O3_1—Ni1'_1—O4_1—C7_1138.07 (13)O7_3—Ni3'_3—O1_3—Ni3_392.3 (18)
O7_1—Ni1'_1—O4_1—C6_1109.35 (15)O6_3—Ni3'_3—O1_3—Ni3_381.2 (17)
O6_1—Ni1'_1—O4_1—C6_171.36 (15)O2_3—Ni3'_3—O1_3—Ni3_3178.7 (18)
O2_1—Ni1'_1—O4_1—C6_133.4 (2)O5_3—Ni3'_3—O1_3—Ni3_37.0 (17)
O1_1—Ni1'_1—O4_1—C6_1163.50 (15)O3_3—Ni3'_3—O1_3—Ni3_3157 (2)
O5_1—Ni1'_1—O4_1—C6_1158.24 (15)O4_3—Ni3'_3—O1_3—Ni3_36.4 (16)
O3_1—Ni1'_1—O4_1—C6_112.36 (13)O7_3—Ni3_3—O1_3—C10_362.08 (16)
O7_1—Ni1'_1—O4_1—Ni1_1110 (2)O6_3—Ni3_3—O1_3—C10_3121.46 (15)
O6_1—Ni1'_1—O4_1—Ni1_171 (2)O3_3—Ni3_3—O1_3—C10_3162.0 (2)
O2_1—Ni1'_1—O4_1—Ni1_134 (2)O5_3—Ni3_3—O1_3—C10_327.95 (15)
O1_1—Ni1'_1—O4_1—Ni1_1163 (2)O4_3—Ni3_3—O1_3—C10_327.5 (3)
O5_1—Ni1'_1—O4_1—Ni1_1158 (2)O2_3—Ni3_3—O1_3—C10_3143.32 (14)
O3_1—Ni1'_1—O4_1—Ni1_113 (2)O7_3—Ni3_3—O1_3—C1_364.11 (17)
O6_1—Ni1_1—O5_1—C8_195.10 (17)O6_3—Ni3_3—O1_3—C1_3112.35 (16)
O7_1—Ni1_1—O5_1—C8_1101.00 (17)O3_3—Ni3_3—O1_3—C1_335.8 (3)
O3_1—Ni1_1—O5_1—C8_19.8 (5)O5_3—Ni3_3—O1_3—C1_3154.14 (14)
O4_1—Ni1_1—O5_1—C8_17.01 (18)O4_3—Ni3_3—O1_3—C1_3153.7 (2)
O2_1—Ni1_1—O5_1—C8_1174.0 (2)O2_3—Ni3_3—O1_3—C1_317.13 (15)
O1_1—Ni1_1—O5_1—C8_1177.72 (15)O7_3—Ni3_3—O1_3—Ni3'_382.5 (18)
O6_1—Ni1_1—O5_1—C9_182.90 (19)O6_3—Ni3_3—O1_3—Ni3'_394.0 (18)
O7_1—Ni1_1—O5_1—C9_180.99 (19)O3_3—Ni3_3—O1_3—Ni3'_317.4 (15)
O3_1—Ni1_1—O5_1—C9_1168.2 (3)O5_3—Ni3_3—O1_3—Ni3'_3172.5 (18)
O4_1—Ni1_1—O5_1—C9_1174.98 (16)O4_3—Ni3_3—O1_3—Ni3'_3172 (2)
O2_1—Ni1_1—O5_1—C9_18.0 (3)O2_3—Ni3_3—O1_3—Ni3'_31.2 (17)
O1_1—Ni1_1—O5_1—C9_10.29 (18)O7_3—Ni3'_3—O2_3—C3_3113.97 (15)
O6_1—Ni1_1—O5_1—Ni1'_185.4 (7)O6_3—Ni3'_3—O2_3—C3_360.01 (18)
O7_1—Ni1_1—O5_1—Ni1'_178.5 (6)O1_3—Ni3'_3—O2_3—C3_3149.30 (14)
O3_1—Ni1_1—O5_1—Ni1'_1170.7 (10)O5_3—Ni3'_3—O2_3—C3_3166.5 (2)
O4_1—Ni1_1—O5_1—Ni1'_1172.5 (7)O3_3—Ni3'_3—O2_3—C3_319.61 (15)
O2_1—Ni1_1—O5_1—Ni1'_15.5 (5)O4_3—Ni3'_3—O2_3—C3_338.7 (2)
O1_1—Ni1_1—O5_1—Ni1'_12.8 (6)O7_3—Ni3'_3—O2_3—C2_3112.82 (15)
O7_1—Ni1'_1—O5_1—C8_189.01 (19)O6_3—Ni3'_3—O2_3—C2_373.20 (17)
O6_1—Ni1'_1—O5_1—C8_183.65 (19)O1_3—Ni3'_3—O2_3—C2_316.09 (15)
O2_1—Ni1'_1—O5_1—C8_1169.5 (2)O5_3—Ni3'_3—O2_3—C2_333.3 (3)
O1_1—Ni1'_1—O5_1—C8_1177.42 (17)O3_3—Ni3'_3—O2_3—C2_3152.82 (14)
O3_1—Ni1'_1—O5_1—C8_15.7 (2)O4_3—Ni3'_3—O2_3—C2_3171.92 (17)
O4_1—Ni1'_1—O5_1—C8_16.11 (16)O7_3—Ni3'_3—O2_3—Ni3_382.5 (10)
O7_1—Ni1'_1—O5_1—C9_192.63 (16)O6_3—Ni3'_3—O2_3—Ni3_391.5 (10)
O6_1—Ni1'_1—O5_1—C9_194.70 (16)O1_3—Ni3'_3—O2_3—Ni3_3179.2 (11)
O2_1—Ni1'_1—O5_1—C9_112.1 (3)O5_3—Ni3'_3—O2_3—Ni3_3162.0 (12)
O1_1—Ni1'_1—O5_1—C9_10.93 (13)O3_3—Ni3'_3—O2_3—Ni3_311.9 (10)
O3_1—Ni1'_1—O5_1—C9_1172.63 (14)O4_3—Ni3'_3—O2_3—Ni3_37.2 (9)
O4_1—Ni1'_1—O5_1—C9_1175.54 (14)O7_3—Ni3_3—O2_3—C3_3120.28 (15)
O7_1—Ni1'_1—O5_1—Ni1_189.6 (7)O6_3—Ni3_3—O2_3—C3_371.42 (17)
O6_1—Ni1'_1—O5_1—Ni1_183.1 (7)O3_3—Ni3_3—O2_3—C3_316.53 (16)
O2_1—Ni1'_1—O5_1—Ni1_1170.0 (8)O5_3—Ni3_3—O2_3—C3_3162.0 (2)
O1_1—Ni1'_1—O5_1—Ni1_1176.9 (7)O4_3—Ni3_3—O2_3—C3_341.0 (4)
O3_1—Ni1'_1—O5_1—Ni1_15.2 (6)O1_3—Ni3_3—O2_3—C3_3150.95 (14)
O4_1—Ni1'_1—O5_1—Ni1_16.7 (6)O7_3—Ni3_3—O2_3—C2_3105.86 (17)
O7_1—Ni1_1—O6_1—Ni1'_110.6 (2)O6_3—Ni3_3—O2_3—C2_362.4 (2)
O3_1—Ni1_1—O6_1—Ni1'_1120.3 (7)O3_3—Ni3_3—O2_3—C2_3150.39 (16)
O4_1—Ni1_1—O6_1—Ni1'_1159.7 (7)O5_3—Ni3_3—O2_3—C2_328.1 (3)
O5_1—Ni1_1—O6_1—Ni1'_187.0 (6)O4_3—Ni3_3—O2_3—C2_3174.9 (3)
O2_1—Ni1_1—O6_1—Ni1'_146.4 (6)O1_3—Ni3_3—O2_3—C2_317.09 (17)
O1_1—Ni1_1—O6_1—Ni1'_119.9 (6)O7_3—Ni3_3—O2_3—Ni3'_389.5 (10)
O2_1—Ni1'_1—O6_1—Ni1_1123.9 (7)O6_3—Ni3_3—O2_3—Ni3'_378.8 (10)
O1_1—Ni1'_1—O6_1—Ni1_1156.5 (7)O3_3—Ni3_3—O2_3—Ni3'_3166.8 (11)
O5_1—Ni1'_1—O6_1—Ni1_182.4 (6)O5_3—Ni3_3—O2_3—Ni3'_311.8 (8)
O3_1—Ni1'_1—O6_1—Ni1_151.1 (6)O4_3—Ni3_3—O2_3—Ni3'_3168.8 (13)
O4_1—Ni1'_1—O6_1—Ni1_116.7 (6)O1_3—Ni3_3—O2_3—Ni3'_30.7 (10)
O2_1—Ni1'_1—O7_1—Ni1_1124.6 (7)O7_3—Ni3_3—O3_3—C4_359.45 (18)
O1_1—Ni1'_1—O7_1—Ni1_1156.3 (7)O6_3—Ni3_3—O3_3—C4_3108.69 (16)
O5_1—Ni1'_1—O7_1—Ni1_182.0 (7)O5_3—Ni3_3—O3_3—C4_3165.3 (3)
O3_1—Ni1'_1—O7_1—Ni1_150.5 (6)O4_3—Ni3_3—O3_3—C4_3151.22 (14)
O4_1—Ni1'_1—O7_1—Ni1_116.5 (6)O2_3—Ni3_3—O3_3—C4_316.98 (17)
O6_1—Ni1_1—O7_1—Ni1'_110.8 (2)O1_3—Ni3_3—O3_3—C4_334.9 (3)
O3_1—Ni1_1—O7_1—Ni1'_1119.0 (7)O7_3—Ni3_3—O3_3—C5_374.19 (18)
O4_1—Ni1_1—O7_1—Ni1'_1160.4 (7)O6_3—Ni3_3—O3_3—C5_3117.67 (15)
O5_1—Ni1_1—O7_1—Ni1'_186.9 (6)O5_3—Ni3_3—O3_3—C5_331.7 (5)
O2_1—Ni1_1—O7_1—Ni1'_147.9 (6)O4_3—Ni3_3—O3_3—C5_317.58 (17)
O1_1—Ni1_1—O7_1—Ni1'_120.1 (6)O2_3—Ni3_3—O3_3—C5_3150.62 (15)
C10_1—O1_1—C1_1—C2_1169.02 (16)O1_3—Ni3_3—O3_3—C5_3168.5 (2)
Ni1'_1—O1_1—C1_1—C2_144.72 (18)O7_3—Ni3_3—O3_3—Ni3'_386.7 (9)
Ni1_1—O1_1—C1_1—C2_145.8 (2)O6_3—Ni3_3—O3_3—Ni3'_381.5 (9)
C3_1—O2_1—C2_1—C1_1178.00 (17)O5_3—Ni3_3—O3_3—Ni3'_3167.5 (13)
Ni1'_1—O2_1—C2_1—C1_144.09 (19)O4_3—Ni3_3—O3_3—Ni3'_3178.4 (10)
Ni1_1—O2_1—C2_1—C1_146.9 (2)O2_3—Ni3_3—O3_3—Ni3'_310.2 (8)
O1_1—C1_1—C2_1—O2_158.5 (2)O1_3—Ni3_3—O3_3—Ni3'_37.6 (7)
C2_1—O2_1—C3_1—C4_1177.87 (17)O7_3—Ni3'_3—O3_3—C4_372.65 (15)
Ni1'_1—O2_1—C3_1—C4_150.4 (2)O6_3—Ni3'_3—O3_3—C4_3116.39 (14)
Ni1_1—O2_1—C3_1—C4_145.9 (2)O2_3—Ni3'_3—O3_3—C4_313.86 (14)
C5_1—O3_1—C4_1—C3_1173.63 (17)O1_3—Ni3'_3—O3_3—C4_338.2 (3)
Ni1_1—O3_1—C4_1—C3_144.0 (2)O5_3—Ni3'_3—O3_3—C4_3162.22 (16)
Ni1'_1—O3_1—C4_1—C3_140.38 (19)O4_3—Ni3'_3—O3_3—C4_3153.15 (13)
O2_1—C3_1—C4_1—O3_157.5 (2)O7_3—Ni3'_3—O3_3—C5_361.27 (18)
C4_1—O3_1—C5_1—C6_1176.71 (17)O6_3—Ni3'_3—O3_3—C5_3109.69 (16)
Ni1_1—O3_1—C5_1—C6_149.1 (2)O2_3—Ni3'_3—O3_3—C5_3147.78 (16)
Ni1'_1—O3_1—C5_1—C6_153.6 (2)O1_3—Ni3'_3—O3_3—C5_3172.2 (2)
C7_1—O4_1—C6_1—C5_1164.24 (17)O5_3—Ni3'_3—O3_3—C5_328.3 (2)
Ni1_1—O4_1—C6_1—C5_142.3 (2)O4_3—Ni3'_3—O3_3—C5_319.23 (15)
Ni1'_1—O4_1—C6_1—C5_142.2 (2)O7_3—Ni3'_3—O3_3—Ni3_381.9 (9)
O3_1—C5_1—C6_1—O4_161.0 (2)O6_3—Ni3'_3—O3_3—Ni3_389.1 (9)
C6_1—O4_1—C7_1—C8_1177.24 (17)O2_3—Ni3'_3—O3_3—Ni3_3168.4 (10)
Ni1_1—O4_1—C7_1—C8_156.0 (2)O1_3—Ni3'_3—O3_3—Ni3_3167.2 (11)
Ni1'_1—O4_1—C7_1—C8_153.09 (18)O5_3—Ni3'_3—O3_3—Ni3_37.7 (8)
C9_1—O5_1—C8_1—C7_1158.38 (17)O4_3—Ni3'_3—O3_3—Ni3_31.4 (9)
Ni1_1—O5_1—C8_1—C7_119.9 (2)O7_3—Ni3_3—O4_3—C7_3120.50 (16)
Ni1'_1—O5_1—C8_1—C7_120.0 (2)O6_3—Ni3_3—O4_3—C7_353.29 (19)
O4_1—C7_1—C8_1—O5_147.9 (2)O3_3—Ni3_3—O4_3—C7_3139.75 (15)
C8_1—O5_1—C9_1—C10_1154.09 (17)O5_3—Ni3_3—O4_3—C7_333.54 (16)
Ni1_1—O5_1—C9_1—C10_127.9 (2)O2_3—Ni3_3—O4_3—C7_3163.7 (3)
Ni1'_1—O5_1—C9_1—C10_127.3 (2)O1_3—Ni3_3—O4_3—C7_334.0 (3)
C1_1—O1_1—C10_1—C9_1177.96 (16)O7_3—Ni3_3—O4_3—C6_3115.00 (17)
Ni1'_1—O1_1—C10_1—C9_154.97 (18)O6_3—Ni3_3—O4_3—C6_371.22 (19)
Ni1_1—O1_1—C10_1—C9_152.40 (19)O3_3—Ni3_3—O4_3—C6_315.24 (17)
O5_1—C9_1—C10_1—O1_151.6 (2)O5_3—Ni3_3—O4_3—C6_3158.05 (15)
O7_2—Ni2'_2—O1_2—C10_257.86 (17)O2_3—Ni3_3—O4_3—C6_339.2 (4)
O6_2—Ni2'_2—O1_2—C10_2114.92 (15)O1_3—Ni3_3—O4_3—C6_3158.5 (2)
O2_2—Ni2'_2—O1_2—C10_2142.90 (14)O7_3—Ni3_3—O4_3—Ni3'_375 (3)
O5_2—Ni2'_2—O1_2—C10_228.66 (15)O6_3—Ni3_3—O4_3—Ni3'_399 (3)
O3_2—Ni2'_2—O1_2—C10_2164.6 (2)O3_3—Ni3_3—O4_3—Ni3'_3175 (3)
O4_2—Ni2'_2—O1_2—C10_227.9 (2)O5_3—Ni3_3—O4_3—Ni3'_312 (3)
O7_2—Ni2'_2—O1_2—C1_267.04 (16)O2_3—Ni3_3—O4_3—Ni3'_3151 (3)
O6_2—Ni2'_2—O1_2—C1_2120.18 (14)O1_3—Ni3_3—O4_3—Ni3'_311 (3)
O2_2—Ni2'_2—O1_2—C1_218.00 (14)O7_3—Ni3'_3—O4_3—C7_3122.81 (14)
O5_2—Ni2'_2—O1_2—C1_2153.56 (13)O6_3—Ni3'_3—O4_3—C7_357.10 (14)
O3_2—Ni2'_2—O1_2—C1_239.7 (3)O2_3—Ni3'_3—O4_3—C7_3160.24 (18)
O4_2—Ni2'_2—O1_2—C1_2152.79 (18)O1_3—Ni3'_3—O4_3—C7_331.9 (2)
O7_2—Ni2'_2—O1_2—Ni2_292 (2)O5_3—Ni3'_3—O4_3—C7_332.51 (13)
O6_2—Ni2'_2—O1_2—Ni2_280 (2)O3_3—Ni3'_3—O4_3—C7_3140.17 (14)
O2_2—Ni2'_2—O1_2—Ni2_2177 (2)O7_3—Ni3'_3—O4_3—C6_3112.24 (15)
O5_2—Ni2'_2—O1_2—Ni2_25.8 (19)O6_3—Ni3'_3—O4_3—C6_367.86 (16)
O3_2—Ni2'_2—O1_2—Ni2_2161 (2)O2_3—Ni3'_3—O4_3—C6_335.3 (2)
O4_2—Ni2'_2—O1_2—Ni2_26.6 (18)O1_3—Ni3'_3—O4_3—C6_3156.82 (18)
O6_2—Ni2_2—O1_2—C10_2118.53 (15)O5_3—Ni3'_3—O4_3—C6_3157.46 (15)
O7_2—Ni2_2—O1_2—C10_263.14 (16)O3_3—Ni3'_3—O4_3—C6_315.22 (14)
O3_2—Ni2_2—O1_2—C10_2161.6 (2)O7_3—Ni3'_3—O4_3—Ni3_3102 (3)
O4_2—Ni2_2—O1_2—C10_225.7 (3)O6_3—Ni3'_3—O4_3—Ni3_378 (3)
O5_2—Ni2_2—O1_2—C10_227.56 (15)O2_3—Ni3'_3—O4_3—Ni3_325 (3)
O2_2—Ni2_2—O1_2—C10_2143.81 (14)O1_3—Ni3'_3—O4_3—Ni3_3167 (3)
O6_2—Ni2_2—O1_2—C1_2116.32 (15)O5_3—Ni3'_3—O4_3—Ni3_3168 (3)
O7_2—Ni2_2—O1_2—C1_262.01 (16)O3_3—Ni3'_3—O4_3—Ni3_35 (3)
O3_2—Ni2_2—O1_2—C1_236.5 (3)O7_3—Ni3_3—O5_3—C8_3100.24 (17)
O4_2—Ni2_2—O1_2—C1_2150.8 (2)O6_3—Ni3_3—O5_3—C8_394.17 (17)
O5_2—Ni2_2—O1_2—C1_2152.71 (14)O3_3—Ni3_3—O5_3—C8_38.5 (5)
O2_2—Ni2_2—O1_2—C1_218.66 (14)O4_3—Ni3_3—O5_3—C8_35.93 (18)
O6_2—Ni2_2—O1_2—Ni2'_295 (2)O2_3—Ni3_3—O5_3—C8_3174.6 (2)
O7_2—Ni2_2—O1_2—Ni2'_283 (2)O1_3—Ni3_3—O5_3—C8_3174.37 (15)
O3_2—Ni2_2—O1_2—Ni2'_215.3 (18)O7_3—Ni3_3—O5_3—C9_387.58 (19)
O4_2—Ni2_2—O1_2—Ni2'_2172 (2)O6_3—Ni3_3—O5_3—C9_378.0 (2)
O5_2—Ni2_2—O1_2—Ni2'_2174 (2)O3_3—Ni3_3—O5_3—C9_3163.7 (3)
O2_2—Ni2_2—O1_2—Ni2'_22.5 (19)O4_3—Ni3_3—O5_3—C9_3178.11 (16)
O7_2—Ni2'_2—O2_2—C2_2110.70 (15)O2_3—Ni3_3—O5_3—C9_313.3 (3)
O6_2—Ni2'_2—O2_2—C2_277.03 (17)O1_3—Ni3_3—O5_3—C9_32.18 (18)
O1_2—Ni2'_2—O2_2—C2_214.52 (15)O7_3—Ni3_3—O5_3—Ni3'_382.4 (8)
O5_2—Ni2'_2—O2_2—C2_233.0 (3)O6_3—Ni3_3—O5_3—Ni3'_383.1 (8)
O3_2—Ni2'_2—O2_2—C2_2154.60 (14)O3_3—Ni3_3—O5_3—Ni3'_3168.8 (11)
O4_2—Ni2'_2—O2_2—C2_2174.21 (17)O4_3—Ni3_3—O5_3—Ni3'_3176.8 (8)
O7_2—Ni2'_2—O2_2—C3_2114.68 (15)O2_3—Ni3_3—O5_3—Ni3'_38.1 (6)
O6_2—Ni2'_2—O2_2—C3_257.58 (18)O1_3—Ni3_3—O5_3—Ni3'_33.0 (7)
O1_2—Ni2'_2—O2_2—C3_2149.13 (15)O7_3—Ni3'_3—O5_3—C8_389.09 (19)
O5_2—Ni2'_2—O2_2—C3_2167.6 (3)O6_3—Ni3'_3—O5_3—C8_382.07 (19)
O3_2—Ni2'_2—O2_2—C3_219.99 (15)O2_3—Ni3'_3—O5_3—C8_3168.7 (2)
O4_2—Ni2'_2—O2_2—C3_239.6 (2)O1_3—Ni3'_3—O5_3—C8_3173.65 (17)
O7_2—Ni2'_2—O2_2—Ni2_282.5 (9)O3_3—Ni3'_3—O5_3—C8_33.3 (3)
O6_2—Ni2'_2—O2_2—Ni2_289.8 (9)O4_3—Ni3'_3—O5_3—C8_35.92 (17)
O1_2—Ni2'_2—O2_2—Ni2_2178.7 (10)O7_3—Ni3'_3—O5_3—C9_398.51 (16)
O5_2—Ni2'_2—O2_2—Ni2_2160.2 (12)O6_3—Ni3'_3—O5_3—C9_390.34 (16)
O3_2—Ni2'_2—O2_2—Ni2_212.2 (9)O2_3—Ni3'_3—O5_3—C9_318.9 (3)
O4_2—Ni2'_2—O2_2—Ni2_27.4 (8)O1_3—Ni3'_3—O5_3—C9_31.24 (15)
O6_2—Ni2_2—O2_2—C2_265.17 (19)O3_3—Ni3'_3—O5_3—C9_3169.14 (15)
O7_2—Ni2_2—O2_2—C2_2103.15 (16)O4_3—Ni3'_3—O5_3—C9_3178.32 (15)
O3_2—Ni2_2—O2_2—C2_2152.21 (15)O7_3—Ni3'_3—O5_3—Ni3_386.1 (8)
O4_2—Ni2_2—O2_2—C2_2177.5 (3)O6_3—Ni3'_3—O5_3—Ni3_385.1 (8)
O5_2—Ni2_2—O2_2—C2_226.5 (3)O2_3—Ni3'_3—O5_3—Ni3_3165.7 (10)
O1_2—Ni2_2—O2_2—C2_215.35 (16)O1_3—Ni3'_3—O5_3—Ni3_3176.7 (8)
O6_2—Ni2_2—O2_2—C3_270.47 (17)O3_3—Ni3'_3—O5_3—Ni3_36.3 (6)
O7_2—Ni2_2—O2_2—C3_2121.21 (15)O4_3—Ni3'_3—O5_3—Ni3_32.9 (7)
O3_2—Ni2_2—O2_2—C3_216.56 (15)O2_3—Ni3'_3—O6_3—Ni3_3127.8 (8)
O4_2—Ni2_2—O2_2—C3_241.9 (4)O1_3—Ni3'_3—O6_3—Ni3_3152.6 (8)
O5_2—Ni2_2—O2_2—C3_2162.1 (2)O5_3—Ni3'_3—O6_3—Ni3_379.1 (8)
O1_2—Ni2_2—O2_2—C3_2151.00 (14)O3_3—Ni3'_3—O6_3—Ni3_354.1 (8)
O6_2—Ni2_2—O2_2—Ni2'_279.4 (9)O4_3—Ni3'_3—O6_3—Ni3_313.4 (7)
O7_2—Ni2_2—O2_2—Ni2'_289.0 (9)O7_3—Ni3_3—O6_3—Ni3'_39.3 (3)
O3_2—Ni2_2—O2_2—Ni2'_2166.4 (10)O3_3—Ni3_3—O6_3—Ni3'_3117.3 (8)
O4_2—Ni2_2—O2_2—Ni2'_2168.3 (12)O5_3—Ni3_3—O6_3—Ni3'_390.1 (8)
O5_2—Ni2_2—O2_2—Ni2'_212.3 (7)O4_3—Ni3_3—O6_3—Ni3'_3163.9 (9)
O1_2—Ni2_2—O2_2—Ni2'_21.2 (9)O2_3—Ni3_3—O6_3—Ni3'_343.2 (7)
O6_2—Ni2_2—O3_2—C4_2110.94 (16)O1_3—Ni3_3—O6_3—Ni3'_323.4 (7)
O7_2—Ni2_2—O3_2—C4_258.87 (18)O2_3—Ni3'_3—O7_3—Ni3_3128.5 (8)
O4_2—Ni2_2—O3_2—C4_2151.39 (14)O1_3—Ni3'_3—O7_3—Ni3_3152.3 (9)
O5_2—Ni2_2—O3_2—C4_2166.0 (3)O5_3—Ni3'_3—O7_3—Ni3_379.2 (8)
O2_2—Ni2_2—O3_2—C4_216.02 (16)O3_3—Ni3'_3—O7_3—Ni3_353.2 (8)
O1_2—Ni2_2—O3_2—C4_233.2 (3)O4_3—Ni3'_3—O7_3—Ni3_313.4 (8)
O6_2—Ni2_2—O3_2—C5_2117.69 (15)O6_3—Ni3_3—O7_3—Ni3'_39.3 (3)
O7_2—Ni2_2—O3_2—C5_272.50 (16)O3_3—Ni3_3—O7_3—Ni3'_3116.1 (8)
O4_2—Ni2_2—O3_2—C5_220.02 (16)O5_3—Ni3_3—O7_3—Ni3'_390.3 (8)
O5_2—Ni2_2—O3_2—C5_234.7 (4)O4_3—Ni3_3—O7_3—Ni3'_3164.2 (9)
O2_2—Ni2_2—O3_2—C5_2147.39 (14)O2_3—Ni3_3—O7_3—Ni3'_344.3 (7)
O1_2—Ni2_2—O3_2—C5_2164.5 (2)O1_3—Ni3_3—O7_3—Ni3'_323.3 (7)
O6_2—Ni2_2—O3_2—Ni2'_283.6 (9)C10_3—O1_3—C1_3—C2_3169.24 (17)
O7_2—Ni2_2—O3_2—Ni2'_286.2 (9)Ni3'_3—O1_3—C1_3—C2_344.3 (2)
O4_2—Ni2_2—O3_2—Ni2'_2178.7 (10)Ni3_3—O1_3—C1_3—C2_345.7 (2)
O5_2—Ni2_2—O3_2—Ni2'_2166.6 (12)C3_3—O2_3—C2_3—C1_3178.69 (17)
O2_2—Ni2_2—O3_2—Ni2'_211.3 (8)Ni3'_3—O2_3—C2_3—C1_344.4 (2)
O1_2—Ni2_2—O3_2—Ni2'_25.8 (7)Ni3_3—O2_3—C2_3—C1_346.8 (2)
O7_2—Ni2'_2—O3_2—C4_272.21 (16)O1_3—C1_3—C2_3—O2_358.3 (2)
O6_2—Ni2'_2—O3_2—C4_2118.56 (14)C2_3—O2_3—C3_3—C4_3179.55 (17)
O2_2—Ni2'_2—O3_2—C4_212.73 (14)Ni3'_3—O2_3—C3_3—C4_348.1 (2)
O1_2—Ni2'_2—O3_2—C4_235.0 (3)Ni3_3—O2_3—C3_3—C4_343.6 (2)
O5_2—Ni2'_2—O3_2—C4_2162.62 (16)C5_3—O3_3—C4_3—C3_3178.31 (17)
O4_2—Ni2'_2—O3_2—C4_2153.40 (13)Ni3_3—O3_3—C4_3—C3_346.2 (2)
O7_2—Ni2'_2—O3_2—C5_259.59 (17)Ni3'_3—O3_3—C4_3—C3_341.75 (18)
O6_2—Ni2'_2—O3_2—C5_2109.64 (16)O2_3—C3_3—C4_3—O3_357.3 (2)
O2_2—Ni2'_2—O3_2—C5_2144.53 (15)C4_3—O3_3—C5_3—C6_3178.55 (17)
O1_2—Ni2'_2—O3_2—C5_2166.8 (2)Ni3_3—O3_3—C5_3—C6_346.3 (2)
O5_2—Ni2'_2—O3_2—C5_230.8 (2)Ni3'_3—O3_3—C5_3—C6_349.8 (2)
O4_2—Ni2'_2—O3_2—C5_221.59 (14)C7_3—O4_3—C6_3—C5_3165.27 (18)
O7_2—Ni2'_2—O3_2—Ni2_282.3 (9)Ni3_3—O4_3—C6_3—C5_343.6 (2)
O6_2—Ni2'_2—O3_2—Ni2_286.9 (9)Ni3'_3—O4_3—C6_3—C5_344.1 (2)
O2_2—Ni2'_2—O3_2—Ni2_2167.3 (9)O3_3—C5_3—C6_3—O4_359.6 (2)
O1_2—Ni2'_2—O3_2—Ni2_2170.5 (11)C6_3—O4_3—C7_3—C8_3176.15 (17)
O5_2—Ni2'_2—O3_2—Ni2_28.1 (8)Ni3_3—O4_3—C7_3—C8_355.1 (2)
O4_2—Ni2'_2—O3_2—Ni2_21.1 (8)Ni3'_3—O4_3—C7_3—C8_353.21 (19)
O6_2—Ni2_2—O4_2—C7_251.54 (18)C9_3—O5_3—C8_3—C7_3152.15 (18)
O7_2—Ni2_2—O4_2—C7_2121.58 (16)Ni3_3—O5_3—C8_3—C7_320.9 (2)
O3_2—Ni2_2—O4_2—C7_2138.63 (14)Ni3'_3—O5_3—C8_3—C7_320.3 (3)
O5_2—Ni2_2—O4_2—C7_234.58 (15)O4_3—C7_3—C8_3—O5_348.5 (2)
O2_2—Ni2_2—O4_2—C7_2163.1 (3)C8_3—O5_3—C9_3—C10_3157.43 (17)
O1_2—Ni2_2—O4_2—C7_236.4 (3)Ni3_3—O5_3—C9_3—C10_330.3 (2)
O6_2—Ni2_2—O4_2—C6_274.06 (18)Ni3'_3—O5_3—C9_3—C10_329.2 (2)
O7_2—Ni2_2—O4_2—C6_2112.82 (16)C1_3—O1_3—C10_3—C9_3176.07 (17)
O3_2—Ni2_2—O4_2—C6_213.04 (16)Ni3'_3—O1_3—C10_3—C9_353.45 (19)
O5_2—Ni2_2—O4_2—C6_2160.17 (14)Ni3_3—O1_3—C10_3—C9_350.71 (19)
O2_2—Ni2_2—O4_2—C6_237.5 (4)O5_3—C9_3—C10_3—O1_351.7 (2)
O1_2—Ni2_2—O4_2—C6_2162.0 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O6_1—H6W1_1···O9_8i0.83 (1)1.90 (1)2.715 (2)165 (2)
O6_1—H6W2_1···O9_70.81 (1)2.22 (2)2.958 (2)151 (2)
O6_1—H6W2_1···O8_70.81 (1)2.27 (1)3.004 (2)150 (2)
O7_1—H7W1_1···O9_6ii0.83 (1)1.97 (1)2.795 (2)170 (2)
O7_1—H7W1_1···O10_6ii0.83 (1)2.45 (2)3.067 (2)132 (2)
O7_1—H7W2_1···O8_40.84 (1)1.88 (1)2.725 (2)175 (2)
O6_2—H6W1_2···O9_4iii0.83 (1)1.93 (1)2.726 (2)162 (2)
O6_2—H6W2_2···O8_50.83 (1)1.93 (1)2.754 (2)175 (2)
O6_2—H6W2_2···O9_50.83 (1)2.57 (2)3.161 (2)129 (2)
O7_2—H7W1_2···O8_80.84 (1)1.90 (1)2.729 (2)171 (2)
O7_2—H7W2_2···O9_9i0.83 (1)1.89 (1)2.715 (2)171 (2)
O7_2—H7W2_2···O10_9i0.83 (1)2.64 (2)3.276 (2)135 (2)
O6_3—H6W1_3···O9_5iii0.83 (1)1.87 (1)2.695 (2)171 (2)
O6_3—H6W2_3···O9_60.83 (1)2.01 (1)2.822 (2)165 (2)
O6_3—H6W2_3···O8_60.83 (1)2.47 (2)3.093 (2)133 (2)
O7_3—H7W1_3···O9_7iv0.83 (1)1.92 (1)2.739 (2)171 (2)
O7_3—H7W1_3···O10_7iv0.83 (1)2.57 (2)3.200 (2)134 (2)
O7_3—H7W2_3···O8_90.83 (1)1.92 (1)2.743 (2)172 (2)
Symmetry codes: (i) x, y+1/2, z1/2; (ii) x, y+3/2, z1/2; (iii) x, y+3/2, z+1/2; (iv) x, y+1/2, z+1/2.
 

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