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
CCDC references: 718168; 718169; 718170; 718171; 718172; 718173; 718174
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.
Crystal data top
C10H20O5·H12NiO62+·2(NO3−)·2(H2O) | F(000) = 1160 |
Mr = 547.12 | Dx = 1.530 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 5679 reflections |
a = 11.950 (1) Å | θ = 1.0–27.5° |
b = 12.686 (1) Å | µ = 0.90 mm−1 |
c = 15.988 (1) Å | T = 90 K |
β = 101.51 (1)° | Parallelepiped, pale green |
V = 2375.0 (3) Å3 | 0.30 × 0.25 × 0.20 mm |
Z = 4 | |
Data collection top
Nonius KappaCCD diffractometer | 5463 independent reflections |
Radiation source: fine-focus sealed tube | 3979 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
Detector resolution: 18 pixels mm-1 | θmax = 27.5°, θmin = 1.7° |
ω scans at fixed χ = 55° | h = −15→15 |
Absorption correction: multi-scan Scalepack (Otwinowski & Minor, 2006) | k = −16→16 |
Tmin = 0.773, Tmax = 0.840 | l = −20→20 |
10666 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.040 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.109 | H 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 parameters | Δρmax = 0.86 e Å−3 |
24 restraints | Δρmin = −0.53 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
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 | x | y | z | Uiso*/Ueq | |
C1 | 0.03958 (19) | 0.14224 (17) | 0.33492 (15) | 0.0211 (5) | |
H1A | 0.0407 | 0.1442 | 0.2732 | 0.025* | |
H1B | −0.0385 | 0.1232 | 0.3417 | 0.025* | |
C2 | 0.1241 (2) | 0.06217 (18) | 0.37905 (15) | 0.0230 (5) | |
H2A | 0.1246 | 0.0615 | 0.4410 | 0.028* | |
H2B | 0.1030 | −0.0091 | 0.3559 | 0.028* | |
C3 | 0.3242 (2) | 0.02237 (17) | 0.40505 (15) | 0.0235 (6) | |
H3A | 0.3239 | −0.0431 | 0.3713 | 0.028* | |
H3B | 0.3128 | 0.0030 | 0.4628 | 0.028* | |
C4 | 0.43581 (19) | 0.07826 (18) | 0.41146 (15) | 0.0224 (5) | |
H4A | 0.4994 | 0.0269 | 0.4229 | 0.027* | |
H4B | 0.4381 | 0.1148 | 0.3571 | 0.027* | |
C5 | 0.5425 (2) | 0.22511 (19) | 0.48578 (16) | 0.0236 (6) | |
H5A | 0.6088 | 0.1865 | 0.4725 | 0.028* | |
H5B | 0.5640 | 0.2516 | 0.5451 | 0.028* | |
C6 | 0.51558 (19) | 0.31702 (18) | 0.42609 (16) | 0.0220 (5) | |
H6A | 0.5823 | 0.3647 | 0.4328 | 0.026* | |
H6B | 0.4978 | 0.2918 | 0.3663 | 0.026* | |
C7 | 0.39404 (19) | 0.46548 (17) | 0.39577 (15) | 0.0203 (5) | |
H7A | 0.4027 | 0.4523 | 0.3364 | 0.024* | |
H7B | 0.4473 | 0.5226 | 0.4198 | 0.024* | |
C8 | 0.27326 (18) | 0.49780 (17) | 0.39676 (14) | 0.0203 (5) | |
H8A | 0.2609 | 0.5007 | 0.4561 | 0.024* | |
H8B | 0.2572 | 0.5683 | 0.3706 | 0.024* | |
C9 | 0.08363 (18) | 0.42862 (18) | 0.35669 (15) | 0.0202 (5) | |
H9A | 0.0476 | 0.4910 | 0.3251 | 0.024* | |
H9B | 0.0784 | 0.4361 | 0.4174 | 0.024* | |
C10 | 0.02372 (19) | 0.32935 (18) | 0.31987 (15) | 0.0208 (5) | |
H10A | −0.0593 | 0.3350 | 0.3184 | 0.025* | |
H10B | 0.0352 | 0.3184 | 0.2608 | 0.025* | |
O1 | 0.07067 (13) | 0.24319 (11) | 0.37265 (10) | 0.0184 (4) | |
O2 | 0.23410 (12) | 0.09047 (12) | 0.36458 (10) | 0.0204 (4) | |
O3 | 0.44751 (13) | 0.15343 (12) | 0.47989 (10) | 0.0200 (4) | |
O4 | 0.41993 (12) | 0.37208 (12) | 0.44538 (10) | 0.0184 (4) | |
O5 | 0.20055 (13) | 0.42081 (12) | 0.34906 (10) | 0.0180 (4) | |
Ni | 0.25925 (2) | 0.24027 (2) | 0.140934 (18) | 0.01200 (10) | |
O6 | 0.28631 (13) | 0.25744 (11) | 0.27029 (10) | 0.0145 (3) | |
H6C | 0.2519 (17) | 0.3101 (9) | 0.2837 (14) | 0.022* | |
H6D | 0.2639 (18) | 0.2072 (10) | 0.2968 (14) | 0.022* | |
O7 | 0.24109 (13) | 0.21594 (13) | 0.01288 (10) | 0.0190 (4) | |
H7C | 0.1933 (14) | 0.2402 (17) | −0.0286 (11) | 0.028* | |
H7D | 0.2997 (12) | 0.2056 (18) | −0.0066 (14) | 0.028* | |
O8 | 0.13210 (12) | 0.13215 (12) | 0.14530 (10) | 0.0161 (3) | |
H8C | 0.1500 (17) | 0.0687 (9) | 0.1505 (14) | 0.024* | |
H8D | 0.0747 (14) | 0.1356 (16) | 0.1059 (11) | 0.024* | |
O9 | 0.37998 (13) | 0.12260 (12) | 0.15538 (10) | 0.0178 (3) | |
H9C | 0.3583 (16) | 0.0608 (9) | 0.1558 (15) | 0.027* | |
H9D | 0.4448 (11) | 0.1264 (16) | 0.1864 (13) | 0.027* | |
O10 | 0.38594 (12) | 0.34916 (12) | 0.13966 (10) | 0.0163 (3) | |
H10C | 0.3934 (17) | 0.3558 (19) | 0.0896 (6) | 0.024* | |
H10D | 0.4506 (11) | 0.3314 (18) | 0.1678 (11) | 0.024* | |
O11 | 0.14051 (12) | 0.35750 (12) | 0.12589 (10) | 0.0170 (3) | |
H11C | 0.1639 (16) | 0.4162 (11) | 0.1126 (14) | 0.025* | |
H11D | 0.0792 (12) | 0.3484 (17) | 0.0907 (12) | 0.025* | |
N1 | 0.65678 (17) | 0.22118 (16) | 0.24141 (13) | 0.0214 (5) | |
O12 | 0.59872 (13) | 0.14155 (13) | 0.25296 (11) | 0.0268 (4) | |
O13 | 0.76169 (14) | 0.21516 (14) | 0.25024 (13) | 0.0357 (5) | |
O14 | 0.60726 (13) | 0.30809 (12) | 0.22190 (11) | 0.0248 (4) | |
N2 | −0.10946 (17) | 0.22812 (15) | −0.00317 (13) | 0.0204 (4) | |
O15 | −0.05771 (13) | 0.14346 (12) | 0.01778 (10) | 0.0234 (4) | |
O16 | −0.20209 (14) | 0.22689 (13) | −0.05639 (12) | 0.0300 (4) | |
O17 | −0.07137 (13) | 0.31451 (12) | 0.02775 (11) | 0.0280 (4) | |
O18 | 0.23536 (16) | 0.54416 (13) | 0.09808 (12) | 0.0295 (4) | |
H18C | 0.262 (2) | 0.5620 (19) | 0.1493 (7) | 0.044* | |
H18D | 0.205 (2) | 0.5999 (13) | 0.0751 (13) | 0.044* | |
O19 | 0.25170 (14) | −0.05515 (12) | 0.16160 (12) | 0.0244 (4) | |
H19C | 0.240 (2) | −0.0924 (16) | 0.1178 (8) | 0.037* | |
H19D | 0.276 (2) | −0.0945 (15) | 0.2029 (9) | 0.037* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0227 (13) | 0.0225 (13) | 0.0198 (13) | −0.0093 (10) | 0.0086 (10) | −0.0071 (10) |
C2 | 0.0311 (14) | 0.0183 (12) | 0.0222 (14) | −0.0062 (10) | 0.0114 (11) | −0.0010 (10) |
C3 | 0.0372 (15) | 0.0149 (12) | 0.0184 (13) | 0.0082 (10) | 0.0053 (11) | 0.0013 (10) |
C4 | 0.0276 (14) | 0.0237 (13) | 0.0174 (13) | 0.0134 (10) | 0.0083 (11) | 0.0036 (10) |
C5 | 0.0131 (12) | 0.0334 (14) | 0.0245 (14) | 0.0005 (10) | 0.0042 (10) | 0.0040 (11) |
C6 | 0.0182 (12) | 0.0247 (13) | 0.0249 (14) | −0.0014 (10) | 0.0087 (10) | 0.0020 (10) |
C7 | 0.0256 (13) | 0.0175 (12) | 0.0185 (13) | −0.0064 (10) | 0.0063 (10) | −0.0002 (10) |
C8 | 0.0293 (14) | 0.0125 (11) | 0.0196 (13) | −0.0029 (10) | 0.0060 (11) | −0.0026 (9) |
C9 | 0.0187 (13) | 0.0204 (12) | 0.0234 (13) | 0.0065 (10) | 0.0089 (10) | 0.0015 (10) |
C10 | 0.0174 (12) | 0.0263 (13) | 0.0185 (13) | 0.0053 (10) | 0.0035 (10) | 0.0039 (10) |
O1 | 0.0198 (9) | 0.0190 (9) | 0.0156 (9) | −0.0013 (6) | 0.0016 (7) | −0.0016 (6) |
O2 | 0.0226 (9) | 0.0184 (9) | 0.0210 (9) | 0.0014 (7) | 0.0060 (7) | 0.0076 (7) |
O3 | 0.0225 (9) | 0.0186 (8) | 0.0213 (9) | 0.0031 (7) | 0.0098 (7) | 0.0014 (7) |
O4 | 0.0164 (8) | 0.0192 (8) | 0.0215 (9) | 0.0007 (6) | 0.0086 (7) | 0.0011 (7) |
O5 | 0.0191 (8) | 0.0165 (8) | 0.0200 (9) | −0.0008 (6) | 0.0077 (7) | −0.0029 (7) |
Ni | 0.01211 (17) | 0.01298 (16) | 0.01132 (17) | −0.00002 (11) | 0.00331 (11) | 0.00008 (11) |
O6 | 0.0166 (9) | 0.0154 (8) | 0.0119 (8) | 0.0015 (6) | 0.0039 (6) | −0.0002 (6) |
O7 | 0.0132 (9) | 0.0327 (9) | 0.0113 (9) | 0.0015 (7) | 0.0029 (7) | −0.0005 (7) |
O8 | 0.0141 (8) | 0.0130 (8) | 0.0198 (9) | −0.0008 (6) | −0.0001 (6) | 0.0023 (7) |
O9 | 0.0129 (8) | 0.0141 (8) | 0.0251 (10) | 0.0018 (6) | 0.0003 (7) | −0.0019 (7) |
O10 | 0.0146 (8) | 0.0176 (8) | 0.0165 (9) | −0.0027 (6) | 0.0027 (7) | 0.0039 (7) |
O11 | 0.0147 (8) | 0.0136 (8) | 0.0220 (9) | 0.0001 (6) | 0.0021 (7) | 0.0012 (7) |
N1 | 0.0204 (12) | 0.0247 (11) | 0.0197 (11) | 0.0001 (8) | 0.0050 (9) | −0.0032 (9) |
O12 | 0.0234 (9) | 0.0191 (9) | 0.0357 (11) | −0.0046 (7) | 0.0010 (8) | −0.0022 (8) |
O13 | 0.0154 (10) | 0.0388 (11) | 0.0521 (13) | −0.0001 (8) | 0.0045 (9) | −0.0090 (9) |
O14 | 0.0221 (9) | 0.0218 (9) | 0.0279 (10) | −0.0007 (7) | −0.0014 (7) | 0.0068 (7) |
N2 | 0.0161 (11) | 0.0255 (11) | 0.0206 (11) | 0.0017 (8) | 0.0060 (9) | −0.0002 (9) |
O15 | 0.0214 (9) | 0.0205 (9) | 0.0265 (10) | 0.0037 (7) | 0.0000 (7) | 0.0067 (7) |
O16 | 0.0182 (10) | 0.0342 (10) | 0.0316 (11) | 0.0081 (7) | −0.0091 (8) | −0.0072 (8) |
O17 | 0.0234 (9) | 0.0208 (9) | 0.0376 (11) | 0.0001 (7) | 0.0005 (8) | −0.0069 (8) |
O18 | 0.0391 (12) | 0.0160 (9) | 0.0347 (11) | 0.0025 (8) | 0.0109 (9) | 0.0031 (8) |
O19 | 0.0244 (10) | 0.0147 (9) | 0.0327 (11) | −0.0003 (7) | 0.0026 (8) | 0.0007 (7) |
Geometric parameters (Å, º) top
C1—O1 | 1.433 (3) | C10—O1 | 1.426 (3) |
C1—C2 | 1.505 (3) | C10—H10A | 0.9900 |
C1—H1A | 0.9900 | C10—H10B | 0.9900 |
C1—H1B | 0.9900 | Ni—O11 | 2.0363 (15) |
C2—O2 | 1.425 (3) | Ni—O7 | 2.0387 (15) |
C2—H2A | 0.9900 | Ni—O6 | 2.0402 (16) |
C2—H2B | 0.9900 | Ni—O10 | 2.0525 (15) |
C3—O2 | 1.430 (3) | Ni—O9 | 2.0566 (14) |
C3—C4 | 1.496 (3) | Ni—O8 | 2.0584 (15) |
C3—H3A | 0.9900 | O6—H6C | 0.835 (9) |
C3—H3B | 0.9900 | O6—H6D | 0.839 (9) |
C4—O3 | 1.437 (3) | O7—H7C | 0.842 (9) |
C4—H4A | 0.9900 | O7—H7D | 0.832 (9) |
C4—H4B | 0.9900 | O8—H8C | 0.833 (9) |
C5—O3 | 1.442 (3) | O8—H8D | 0.835 (9) |
C5—C6 | 1.500 (3) | O9—H9C | 0.826 (9) |
C5—H5A | 0.9900 | O9—H9D | 0.833 (9) |
C5—H5B | 0.9900 | O10—H10C | 0.826 (9) |
C6—O4 | 1.425 (3) | O10—H10D | 0.844 (9) |
C6—H6A | 0.9900 | O11—H11C | 0.837 (9) |
C6—H6B | 0.9900 | O11—H11D | 0.837 (9) |
C7—O4 | 1.425 (3) | N1—O13 | 1.236 (2) |
C7—C8 | 1.504 (3) | N1—O12 | 1.260 (2) |
C7—H7A | 0.9900 | N1—O14 | 1.261 (2) |
C7—H7B | 0.9900 | N2—O17 | 1.250 (2) |
C8—O5 | 1.423 (3) | N2—O15 | 1.251 (2) |
C8—H8A | 0.9900 | N2—O16 | 1.254 (3) |
C8—H8B | 0.9900 | O18—H18C | 0.849 (9) |
C9—O5 | 1.430 (2) | O18—H18D | 0.842 (9) |
C9—C10 | 1.509 (3) | O19—H19C | 0.834 (9) |
C9—H9A | 0.9900 | O19—H19D | 0.832 (9) |
C9—H9B | 0.9900 | | |
| | | |
O1—C1—C2 | 108.20 (18) | H9A—C9—H9B | 108.5 |
O1—C1—H1A | 110.1 | O1—C10—C9 | 107.99 (18) |
C2—C1—H1A | 110.1 | O1—C10—H10A | 110.1 |
O1—C1—H1B | 110.1 | C9—C10—H10A | 110.1 |
C2—C1—H1B | 110.1 | O1—C10—H10B | 110.1 |
H1A—C1—H1B | 108.4 | C9—C10—H10B | 110.1 |
O2—C2—C1 | 107.96 (17) | H10A—C10—H10B | 108.4 |
O2—C2—H2A | 110.1 | C10—O1—C1 | 113.44 (18) |
C1—C2—H2A | 110.1 | C2—O2—C3 | 114.18 (17) |
O2—C2—H2B | 110.1 | C4—O3—C5 | 115.08 (16) |
C1—C2—H2B | 110.1 | C6—O4—C7 | 112.43 (16) |
H2A—C2—H2B | 108.4 | C8—O5—C9 | 114.15 (16) |
O2—C3—C4 | 108.96 (18) | O11—Ni—O7 | 93.43 (7) |
O2—C3—H3A | 109.9 | O11—Ni—O6 | 90.43 (6) |
C4—C3—H3A | 109.9 | O7—Ni—O6 | 176.12 (6) |
O2—C3—H3B | 109.9 | O11—Ni—O10 | 90.30 (6) |
C4—C3—H3B | 109.9 | O7—Ni—O10 | 91.31 (6) |
H3A—C3—H3B | 108.3 | O6—Ni—O10 | 88.29 (6) |
O3—C4—C3 | 108.46 (17) | O11—Ni—O9 | 179.47 (6) |
O3—C4—H4A | 110.0 | O7—Ni—O9 | 86.25 (7) |
C3—C4—H4A | 110.0 | O6—Ni—O9 | 89.88 (6) |
O3—C4—H4B | 110.0 | O10—Ni—O9 | 89.27 (6) |
C3—C4—H4B | 110.0 | O11—Ni—O8 | 89.37 (6) |
H4A—C4—H4B | 108.4 | O7—Ni—O8 | 90.10 (6) |
O3—C5—C6 | 112.50 (19) | O6—Ni—O8 | 90.32 (6) |
O3—C5—H5A | 109.1 | O10—Ni—O8 | 178.57 (6) |
C6—C5—H5A | 109.1 | O9—Ni—O8 | 91.07 (6) |
O3—C5—H5B | 109.1 | Ni—O6—H6C | 111.0 (16) |
C6—C5—H5B | 109.1 | Ni—O6—H6D | 115.4 (16) |
H5A—C5—H5B | 107.8 | H6C—O6—H6D | 104.8 (14) |
O4—C6—C5 | 108.81 (18) | Ni—O7—H7C | 130.9 (16) |
O4—C6—H6A | 109.9 | Ni—O7—H7D | 118.1 (16) |
C5—C6—H6A | 109.9 | H7C—O7—H7D | 104.6 (14) |
O4—C6—H6B | 109.9 | Ni—O8—H8C | 118.1 (15) |
C5—C6—H6B | 109.9 | Ni—O8—H8D | 116.1 (16) |
H6A—C6—H6B | 108.3 | H8C—O8—H8D | 106.4 (14) |
O4—C7—C8 | 108.85 (17) | Ni—O9—H9C | 118.4 (15) |
O4—C7—H7A | 109.9 | Ni—O9—H9D | 124.9 (15) |
C8—C7—H7A | 109.9 | H9C—O9—H9D | 107.9 (14) |
O4—C7—H7B | 109.9 | Ni—O10—H10C | 107.5 (16) |
C8—C7—H7B | 109.9 | Ni—O10—H10D | 114.5 (16) |
H7A—C7—H7B | 108.3 | H10C—O10—H10D | 106.2 (13) |
O5—C8—C7 | 106.97 (17) | Ni—O11—H11C | 114.8 (15) |
O5—C8—H8A | 110.3 | Ni—O11—H11D | 118.3 (16) |
C7—C8—H8A | 110.3 | H11C—O11—H11D | 104.1 (14) |
O5—C8—H8B | 110.3 | O13—N1—O12 | 120.6 (2) |
C7—C8—H8B | 110.3 | O13—N1—O14 | 119.9 (2) |
H8A—C8—H8B | 108.6 | O12—N1—O14 | 119.50 (19) |
O5—C9—C10 | 107.73 (17) | O17—N2—O15 | 121.7 (2) |
O5—C9—H9A | 110.2 | O17—N2—O16 | 118.78 (19) |
C10—C9—H9A | 110.2 | O15—N2—O16 | 119.54 (19) |
O5—C9—H9B | 110.2 | H18C—O18—H18D | 104.1 (14) |
C10—C9—H9B | 110.2 | H19C—O19—H19D | 107.5 (15) |
| | | |
O1—C1—C2—O2 | −62.1 (2) | C4—C3—O2—C2 | −160.60 (18) |
O2—C3—C4—O3 | 76.5 (2) | C3—C4—O3—C5 | −170.80 (18) |
O3—C5—C6—O4 | 58.7 (3) | C6—C5—O3—C4 | 82.7 (2) |
O4—C7—C8—O5 | −68.9 (2) | C5—C6—O4—C7 | 175.50 (19) |
O5—C9—C10—O1 | 65.7 (2) | C8—C7—O4—C6 | 160.76 (18) |
C9—C10—O1—C1 | −167.05 (17) | C7—C8—O5—C9 | 168.99 (17) |
C2—C1—O1—C10 | 159.91 (17) | C10—C9—O5—C8 | −167.49 (18) |
C1—C2—O2—C3 | 178.40 (18) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O6—H6D···O2 | 0.84 (1) | 1.91 (1) | 2.743 (2) | 172 (2) |
O6—H6C···O5 | 0.84 (1) | 1.92 (1) | 2.729 (2) | 162 (2) |
O7—H7C···O1i | 0.84 (1) | 1.94 (1) | 2.761 (2) | 165 (2) |
O7—H7D···O3i | 0.83 (1) | 2.55 (2) | 3.103 (2) | 125 (2) |
O7—H7D···O4i | 0.83 (1) | 2.02 (1) | 2.811 (2) | 160 (2) |
O8—H8D···O15 | 0.84 (1) | 1.90 (1) | 2.734 (2) | 179 (2) |
O8—H8C···O19 | 0.83 (1) | 1.97 (1) | 2.758 (2) | 157 (2) |
O9—H9D···O12 | 0.83 (1) | 1.94 (1) | 2.774 (2) | 176 (2) |
O9—H9C···O19 | 0.83 (1) | 1.96 (1) | 2.740 (2) | 157 (2) |
O10—H10C···O3i | 0.83 (1) | 1.99 (1) | 2.796 (2) | 164 (2) |
O10—H10D···O14 | 0.84 (1) | 1.92 (1) | 2.758 (2) | 171 (2) |
O11—H11D···O17 | 0.84 (1) | 1.93 (1) | 2.754 (2) | 169 (2) |
O11—H11C···O18 | 0.84 (1) | 1.87 (1) | 2.700 (2) | 171 (2) |
O18—H18C···O12ii | 0.85 (1) | 2.28 (2) | 3.041 (2) | 150 (2) |
O18—H18C···O13ii | 0.85 (1) | 2.57 (2) | 3.249 (3) | 137 (2) |
O18—H18D···O16iii | 0.84 (1) | 2.22 (2) | 2.989 (2) | 152 (2) |
O18—H18D···O17iii | 0.84 (1) | 2.32 (1) | 3.087 (2) | 151 (2) |
O19—H19D···O13iv | 0.83 (1) | 2.59 (2) | 3.255 (2) | 137 (2) |
O19—H19D···O14iv | 0.83 (1) | 2.06 (1) | 2.840 (2) | 155 (2) |
O19—H19C···O16v | 0.83 (1) | 1.98 (2) | 2.744 (2) | 153 (2) |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) −x+1, y+1/2, −z+1/2; (iii) −x, −y+1, −z; (iv) −x+1, y−1/2, −z+1/2; (v) −x, −y, −z. |
Crystal data top
C10H20O5·H12NiO62+·2(NO3−)·H2O | F(000) = 2240 |
Mr = 529.10 | Dx = 1.535 Mg m−3 |
Monoclinic, B21 | Mo Kα radiation, λ = 0.71073 Å |
a = 16.176 (2) Å | Cell parameters from 5425 reflections |
b = 16.514 (2) Å | θ = 1.0–27.5° |
c = 17.876 (2) Å | µ = 0.93 mm−1 |
β = 106.42 (1)° | T = 90 K |
V = 4580.5 (10) Å3 | Parallelepiped, pale green |
Z = 8 | 0.40 × 0.20 × 0.20 mm |
Data collection top
Nonius KappaCCD diffractometer | 10301 independent reflections |
Radiation source: fine-focus sealed tube | 8534 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.000 |
Detector resolution: 18 pixels mm-1 | θmax = 27.5°, θmin = 1.5° |
ω scans at fixed χ = 55° | h = −20→20 |
Absorption correction: multi-scan Scalepack (Otwinowski & Minor, 2006) | k = −21→20 |
Tmin = 0.707, Tmax = 0.836 | l = −23→23 |
10301 measured reflections | |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H 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 = 1.04 | Δρmax = 0.58 e Å−3 |
10301 reflections | Δρmin = −0.41 e Å−3 |
648 parameters | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
43 restraints | Extinction coefficient: 0.00036 (6) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Secondary atom site location: difference Fourier map | Absolute 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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C1_1 | 0.04439 (17) | 0.18343 (16) | 0.05096 (13) | 0.0231 (6) | |
H1A_1 | 0.0051 | 0.1409 | 0.0218 | 0.028* | |
H1B_1 | 0.1041 | 0.1689 | 0.0521 | 0.028* | |
C2_1 | 0.02062 (15) | 0.26447 (16) | 0.01186 (14) | 0.0215 (6) | |
H2A_1 | 0.0074 | 0.2581 | −0.0454 | 0.026* | |
H2B_1 | −0.0314 | 0.2859 | 0.0238 | 0.026* | |
C3_1 | 0.06835 (16) | 0.40306 (16) | 0.01996 (13) | 0.0229 (6) | |
H3A_1 | 0.0286 | 0.4060 | −0.0335 | 0.027* | |
H3B_1 | 0.1211 | 0.4338 | 0.0205 | 0.027* | |
C4_1 | 0.02621 (15) | 0.44161 (16) | 0.07578 (14) | 0.0218 (5) | |
H4A_1 | 0.0133 | 0.4992 | 0.0618 | 0.026* | |
H4B_1 | −0.0285 | 0.4136 | 0.0735 | 0.026* | |
C5_1 | 0.05249 (16) | 0.47752 (16) | 0.20859 (14) | 0.0192 (6) | |
H5A_1 | −0.0096 | 0.4660 | 0.1997 | 0.023* | |
H5B_1 | 0.0596 | 0.5366 | 0.2036 | 0.023* | |
C6_1 | 0.10217 (15) | 0.44992 (15) | 0.28862 (14) | 0.0203 (5) | |
H6A_1 | 0.1648 | 0.4516 | 0.2941 | 0.024* | |
H6B_1 | 0.0902 | 0.4860 | 0.3285 | 0.024* | |
C7_1 | 0.13483 (15) | 0.32544 (15) | 0.36078 (13) | 0.0192 (6) | |
H7A_1 | 0.1342 | 0.3482 | 0.4118 | 0.023* | |
H7B_1 | 0.1941 | 0.3300 | 0.3559 | 0.023* | |
C8_1 | 0.10753 (16) | 0.23881 (16) | 0.35541 (14) | 0.0207 (5) | |
H8A_1 | 0.1428 | 0.2084 | 0.4011 | 0.025* | |
H8B_1 | 0.0463 | 0.2348 | 0.3550 | 0.025* | |
C9_1 | 0.06617 (16) | 0.13652 (15) | 0.25657 (14) | 0.0202 (6) | |
H9A_1 | 0.0059 | 0.1474 | 0.2562 | 0.024* | |
H9B_1 | 0.0873 | 0.0891 | 0.2904 | 0.024* | |
C10_1 | 0.07072 (16) | 0.12003 (16) | 0.17554 (15) | 0.0235 (6) | |
H10A_1 | 0.1312 | 0.1101 | 0.1759 | 0.028* | |
H10B_1 | 0.0363 | 0.0714 | 0.1543 | 0.028* | |
O1_1 | 0.03728 (10) | 0.18919 (10) | 0.12830 (9) | 0.0189 (4) | |
O2_1 | 0.09079 (10) | 0.32002 (11) | 0.03908 (9) | 0.0202 (4) | |
O3_1 | 0.08397 (10) | 0.43561 (10) | 0.15234 (9) | 0.0184 (4) | |
O4_1 | 0.07606 (10) | 0.36869 (10) | 0.29909 (9) | 0.0185 (4) | |
O5_1 | 0.11873 (10) | 0.20532 (10) | 0.28515 (9) | 0.0184 (4) | |
Ni1_1 | 0.325421 (16) | 0.301237 (17) | 0.198968 (14) | 0.00986 (7) | |
O6_1 | 0.20285 (9) | 0.30515 (12) | 0.20931 (9) | 0.0155 (3) | |
H6C_1 | 0.1676 (12) | 0.3409 (10) | 0.1890 (14) | 0.023* | |
H6D_1 | 0.1747 (13) | 0.2715 (11) | 0.2273 (14) | 0.023* | |
O7_1 | 0.44503 (9) | 0.30994 (10) | 0.18265 (8) | 0.0130 (3) | |
H7C_1 | 0.4853 (11) | 0.3179 (14) | 0.2228 (8) | 0.020* | |
H7D_1 | 0.4651 (13) | 0.2767 (12) | 0.1568 (11) | 0.020* | |
O8_1 | 0.27377 (10) | 0.32585 (10) | 0.08305 (9) | 0.0161 (3) | |
H8C_1 | 0.2209 (6) | 0.3210 (14) | 0.0650 (13) | 0.024* | |
H8D_1 | 0.2882 (13) | 0.3606 (13) | 0.0548 (12) | 0.024* | |
O9_1 | 0.34170 (10) | 0.42168 (9) | 0.23208 (9) | 0.0153 (3) | |
H9C_1 | 0.3136 (14) | 0.4515 (13) | 0.1966 (9) | 0.023* | |
H9D_1 | 0.3282 (15) | 0.4371 (15) | 0.2719 (8) | 0.023* | |
O10_1 | 0.37385 (10) | 0.26884 (10) | 0.31447 (8) | 0.0140 (3) | |
H10C_1 | 0.3700 (15) | 0.3042 (9) | 0.3478 (11) | 0.021* | |
H10D_1 | 0.3584 (16) | 0.2261 (8) | 0.3337 (13) | 0.021* | |
O11_1 | 0.32119 (10) | 0.18011 (10) | 0.17230 (9) | 0.0159 (3) | |
H11C_1 | 0.2959 (15) | 0.1557 (14) | 0.1999 (10) | 0.024* | |
H11D_1 | 0.3012 (15) | 0.1617 (14) | 0.1273 (7) | 0.024* | |
N1_1 | 0.32437 (11) | 0.43406 (12) | 0.43286 (10) | 0.0143 (4) | |
O12_1 | 0.35105 (11) | 0.36294 (10) | 0.43343 (9) | 0.0211 (4) | |
O13_1 | 0.30140 (11) | 0.45917 (10) | 0.49027 (9) | 0.0213 (4) | |
O14_1 | 0.31961 (12) | 0.47919 (11) | 0.37612 (10) | 0.0239 (4) | |
N2_1 | 0.28287 (13) | 0.08032 (12) | 0.34666 (11) | 0.0187 (4) | |
O15_1 | 0.27197 (10) | 0.07636 (10) | 0.27462 (8) | 0.0174 (4) | |
O16_1 | 0.24559 (11) | 0.03107 (10) | 0.37932 (9) | 0.0237 (4) | |
O17_1 | 0.33073 (13) | 0.13364 (11) | 0.38673 (10) | 0.0310 (5) | |
O18_1 | 0.2562 (3) | 0.1252 (2) | 0.02488 (16) | 0.0294 (9) | 0.809 (9) |
O18'_1 | 0.2987 (12) | 0.1052 (9) | 0.0363 (8) | 0.0294 (9) | 0.191 (9) |
H18C_1 | 0.2860 (19) | 0.1292 (16) | −0.0066 (16) | 0.044* | |
H18D_1 | 0.2439 (19) | 0.0758 (8) | 0.0235 (17) | 0.044* | |
C1_2 | 0.53107 (16) | 0.22805 (16) | 0.02330 (13) | 0.0214 (5) | |
H1A_2 | 0.4868 | 0.1961 | −0.0149 | 0.026* | |
H1B_2 | 0.5884 | 0.2127 | 0.0183 | 0.026* | |
C2_2 | 0.51571 (14) | 0.31704 (15) | 0.00768 (13) | 0.0178 (5) | |
H2A_2 | 0.4993 | 0.3272 | −0.0492 | 0.021* | |
H2B_2 | 0.4680 | 0.3356 | 0.0280 | 0.021* | |
C3_2 | 0.57909 (16) | 0.44617 (15) | 0.04688 (14) | 0.0230 (6) | |
H3A_2 | 0.5392 | 0.4636 | −0.0034 | 0.028* | |
H3B_2 | 0.6347 | 0.4744 | 0.0535 | 0.028* | |
C4_2 | 0.54211 (16) | 0.47005 (16) | 0.11259 (14) | 0.0226 (6) | |
H4A_2 | 0.5373 | 0.5297 | 0.1149 | 0.027* | |
H4B_2 | 0.4839 | 0.4464 | 0.1040 | 0.027* | |
C5_2 | 0.57666 (16) | 0.46905 (16) | 0.25100 (14) | 0.0203 (6) | |
H5A_2 | 0.5136 | 0.4653 | 0.2426 | 0.024* | |
H5B_2 | 0.5939 | 0.5265 | 0.2608 | 0.024* | |
C6_2 | 0.62248 (15) | 0.41848 (15) | 0.31943 (13) | 0.0211 (5) | |
H6A_2 | 0.6837 | 0.4119 | 0.3208 | 0.025* | |
H6B_2 | 0.6201 | 0.4450 | 0.3684 | 0.025* | |
C7_2 | 0.63007 (15) | 0.27862 (16) | 0.36054 (13) | 0.0200 (6) | |
H7A_2 | 0.6296 | 0.2866 | 0.4153 | 0.024* | |
H7B_2 | 0.6906 | 0.2799 | 0.3586 | 0.024* | |
C8_2 | 0.58956 (16) | 0.19899 (16) | 0.33080 (13) | 0.0199 (5) | |
H8A_2 | 0.6157 | 0.1549 | 0.3674 | 0.024* | |
H8B_2 | 0.5269 | 0.2004 | 0.3250 | 0.024* | |
C9_2 | 0.55234 (16) | 0.12473 (15) | 0.20976 (14) | 0.0177 (5) | |
H9A_2 | 0.4917 | 0.1312 | 0.2104 | 0.021* | |
H9B_2 | 0.5725 | 0.0704 | 0.2304 | 0.021* | |
C10_2 | 0.55897 (16) | 0.13350 (15) | 0.12790 (14) | 0.0189 (5) | |
H10A_2 | 0.6197 | 0.1281 | 0.1273 | 0.023* | |
H10B_2 | 0.5245 | 0.0910 | 0.0940 | 0.023* | |
O1_2 | 0.52681 (10) | 0.21182 (10) | 0.10056 (9) | 0.0181 (4) | |
O2_2 | 0.59253 (10) | 0.36047 (11) | 0.04492 (9) | 0.0193 (4) | |
O3_2 | 0.59857 (10) | 0.44038 (10) | 0.18339 (9) | 0.0185 (4) | |
O4_2 | 0.58130 (10) | 0.34137 (10) | 0.31210 (9) | 0.0181 (4) | |
O5_2 | 0.60505 (10) | 0.18609 (10) | 0.25677 (9) | 0.0170 (3) | |
Ni2_2 | 0.825118 (16) | 0.297252 (17) | 0.196959 (14) | 0.00979 (7) | |
O6_2 | 0.70295 (9) | 0.30002 (12) | 0.20898 (9) | 0.0145 (3) | |
H6C_2 | 0.6706 (13) | 0.3395 (9) | 0.1940 (14) | 0.022* | |
H6D_2 | 0.6730 (13) | 0.2655 (10) | 0.2225 (14) | 0.022* | |
O7_2 | 0.94396 (9) | 0.30420 (11) | 0.17956 (8) | 0.0124 (3) | |
H7C_2 | 0.9844 (11) | 0.3188 (13) | 0.2183 (9) | 0.019* | |
H7D_2 | 0.9673 (13) | 0.2658 (11) | 0.1615 (12) | 0.019* | |
O8_2 | 0.77091 (10) | 0.32865 (10) | 0.08252 (9) | 0.0150 (3) | |
H8C_2 | 0.7180 (6) | 0.3368 (14) | 0.0701 (14) | 0.022* | |
H8D_2 | 0.7905 (12) | 0.3657 (12) | 0.0605 (13) | 0.022* | |
O9_2 | 0.84586 (10) | 0.41468 (9) | 0.23555 (9) | 0.0149 (3) | |
H9C_2 | 0.8200 (15) | 0.4487 (12) | 0.2029 (9) | 0.022* | |
H9D_2 | 0.8410 (15) | 0.4301 (14) | 0.2783 (7) | 0.022* | |
O10_2 | 0.87546 (10) | 0.26236 (10) | 0.31186 (9) | 0.0139 (3) | |
H10C_2 | 0.8635 (15) | 0.2965 (10) | 0.3426 (12) | 0.021* | |
H10D_2 | 0.8569 (15) | 0.2187 (8) | 0.3254 (13) | 0.021* | |
O11_2 | 0.81789 (10) | 0.17723 (10) | 0.16744 (9) | 0.0153 (3) | |
H11C_2 | 0.7946 (15) | 0.1490 (14) | 0.1951 (10) | 0.023* | |
H11D_2 | 0.7942 (14) | 0.1609 (14) | 0.1218 (6) | 0.023* | |
N1_2 | 0.83228 (12) | 0.42409 (12) | 0.43458 (10) | 0.0163 (4) | |
O12_2 | 0.82528 (10) | 0.34915 (10) | 0.42234 (9) | 0.0182 (4) | |
O13_2 | 0.81966 (12) | 0.45213 (10) | 0.49524 (9) | 0.0235 (4) | |
O14_2 | 0.85093 (13) | 0.46915 (11) | 0.38624 (10) | 0.0319 (5) | |
N2_2 | 0.76602 (12) | 0.08139 (11) | 0.33450 (11) | 0.0163 (4) | |
O15_2 | 0.75992 (10) | 0.07435 (9) | 0.26371 (9) | 0.0182 (4) | |
O16_2 | 0.72429 (11) | 0.03497 (10) | 0.36583 (9) | 0.0204 (4) | |
O17_2 | 0.81366 (12) | 0.13438 (11) | 0.37563 (10) | 0.0270 (4) | |
O18_2 | 0.74373 (15) | 0.11927 (12) | 0.02295 (11) | 0.0358 (5) | |
H18C_2 | 0.7836 (16) | 0.1172 (17) | −0.0001 (19) | 0.054* | |
H18D_2 | 0.7251 (18) | 0.0712 (9) | 0.0173 (18) | 0.054* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1_1 | 0.0232 (14) | 0.0287 (14) | 0.0172 (12) | 0.0007 (11) | 0.0056 (10) | −0.0094 (11) |
C2_1 | 0.0157 (13) | 0.0340 (15) | 0.0140 (12) | 0.0001 (11) | 0.0031 (10) | −0.0031 (11) |
C3_1 | 0.0215 (13) | 0.0300 (15) | 0.0167 (12) | 0.0029 (11) | 0.0047 (10) | 0.0074 (11) |
C4_1 | 0.0178 (13) | 0.0233 (13) | 0.0231 (13) | 0.0061 (11) | 0.0039 (10) | 0.0052 (11) |
C5_1 | 0.0182 (13) | 0.0158 (13) | 0.0261 (14) | −0.0006 (11) | 0.0102 (11) | −0.0057 (11) |
C6_1 | 0.0176 (12) | 0.0216 (13) | 0.0236 (13) | −0.0069 (10) | 0.0088 (10) | −0.0079 (11) |
C7_1 | 0.0140 (13) | 0.0302 (15) | 0.0121 (11) | 0.0012 (10) | 0.0015 (10) | −0.0020 (10) |
C8_1 | 0.0195 (13) | 0.0295 (14) | 0.0148 (12) | 0.0042 (11) | 0.0077 (10) | 0.0029 (11) |
C9_1 | 0.0183 (13) | 0.0132 (13) | 0.0279 (14) | −0.0023 (10) | 0.0045 (11) | 0.0037 (11) |
C10_1 | 0.0208 (13) | 0.0159 (13) | 0.0311 (14) | 0.0031 (11) | 0.0029 (11) | −0.0012 (11) |
O1_1 | 0.0188 (9) | 0.0197 (9) | 0.0196 (8) | 0.0047 (7) | 0.0076 (7) | −0.0031 (7) |
O2_1 | 0.0144 (8) | 0.0295 (10) | 0.0154 (8) | 0.0013 (7) | 0.0021 (7) | −0.0011 (7) |
O3_1 | 0.0153 (9) | 0.0217 (9) | 0.0177 (8) | 0.0037 (7) | 0.0042 (7) | 0.0002 (7) |
O4_1 | 0.0135 (8) | 0.0224 (9) | 0.0184 (9) | −0.0036 (7) | 0.0025 (7) | −0.0007 (7) |
O5_1 | 0.0189 (9) | 0.0191 (9) | 0.0194 (8) | −0.0027 (7) | 0.0090 (7) | 0.0008 (7) |
Ni1_1 | 0.00909 (14) | 0.01140 (15) | 0.00932 (13) | −0.00030 (12) | 0.00296 (10) | 0.00000 (12) |
O6_1 | 0.0088 (8) | 0.0213 (9) | 0.0178 (8) | 0.0016 (8) | 0.0060 (6) | 0.0070 (8) |
O7_1 | 0.0088 (7) | 0.0175 (10) | 0.0134 (7) | 0.0010 (7) | 0.0040 (6) | −0.0024 (7) |
O8_1 | 0.0141 (8) | 0.0217 (9) | 0.0124 (8) | −0.0018 (7) | 0.0032 (7) | 0.0045 (7) |
O9_1 | 0.0183 (8) | 0.0137 (8) | 0.0149 (8) | 0.0013 (7) | 0.0064 (7) | −0.0004 (7) |
O10_1 | 0.0164 (8) | 0.0155 (8) | 0.0091 (7) | 0.0012 (7) | 0.0022 (6) | −0.0002 (6) |
O11_1 | 0.0230 (9) | 0.0121 (8) | 0.0138 (8) | −0.0039 (7) | 0.0070 (7) | −0.0010 (7) |
N1_1 | 0.0125 (10) | 0.0177 (11) | 0.0124 (9) | −0.0045 (8) | 0.0029 (8) | −0.0019 (8) |
O12_1 | 0.0277 (10) | 0.0169 (9) | 0.0173 (8) | 0.0105 (8) | 0.0039 (7) | 0.0007 (7) |
O13_1 | 0.0315 (10) | 0.0203 (9) | 0.0155 (8) | 0.0050 (8) | 0.0120 (7) | 0.0014 (7) |
O14_1 | 0.0376 (11) | 0.0205 (10) | 0.0156 (9) | −0.0019 (8) | 0.0106 (8) | 0.0034 (8) |
N2_1 | 0.0215 (11) | 0.0158 (11) | 0.0191 (11) | −0.0006 (9) | 0.0065 (9) | 0.0009 (9) |
O15_1 | 0.0217 (9) | 0.0195 (9) | 0.0125 (8) | 0.0006 (7) | 0.0074 (7) | 0.0012 (7) |
O16_1 | 0.0364 (11) | 0.0197 (9) | 0.0199 (9) | −0.0088 (8) | 0.0159 (8) | −0.0003 (7) |
O17_1 | 0.0461 (12) | 0.0210 (10) | 0.0207 (10) | −0.0171 (9) | 0.0011 (9) | −0.0019 (8) |
O18_1 | 0.048 (3) | 0.0225 (15) | 0.0205 (12) | −0.0138 (15) | 0.0145 (15) | −0.0064 (11) |
O18'_1 | 0.048 (3) | 0.0225 (15) | 0.0205 (12) | −0.0138 (15) | 0.0145 (15) | −0.0064 (11) |
C1_2 | 0.0221 (13) | 0.0279 (14) | 0.0144 (12) | −0.0022 (11) | 0.0056 (10) | −0.0051 (10) |
C2_2 | 0.0105 (12) | 0.0260 (14) | 0.0141 (11) | −0.0015 (10) | −0.0011 (9) | 0.0009 (10) |
C3_2 | 0.0243 (14) | 0.0219 (13) | 0.0201 (12) | 0.0012 (11) | 0.0020 (10) | 0.0079 (11) |
C4_2 | 0.0178 (13) | 0.0196 (13) | 0.0262 (13) | 0.0052 (10) | −0.0004 (10) | 0.0046 (11) |
C5_2 | 0.0154 (13) | 0.0169 (13) | 0.0310 (15) | −0.0010 (10) | 0.0106 (11) | −0.0072 (11) |
C6_2 | 0.0167 (12) | 0.0241 (14) | 0.0227 (13) | −0.0055 (10) | 0.0060 (10) | −0.0086 (11) |
C7_2 | 0.0151 (12) | 0.0326 (17) | 0.0121 (11) | 0.0037 (11) | 0.0037 (9) | 0.0017 (11) |
C8_2 | 0.0189 (12) | 0.0267 (14) | 0.0160 (12) | 0.0011 (11) | 0.0082 (10) | 0.0033 (11) |
C9_2 | 0.0168 (13) | 0.0106 (12) | 0.0245 (13) | −0.0019 (10) | 0.0039 (11) | 0.0016 (11) |
C10_2 | 0.0194 (13) | 0.0134 (12) | 0.0246 (13) | 0.0029 (10) | 0.0072 (11) | −0.0026 (11) |
O1_2 | 0.0206 (9) | 0.0192 (9) | 0.0165 (8) | 0.0032 (7) | 0.0084 (7) | −0.0015 (7) |
O2_2 | 0.0156 (9) | 0.0230 (9) | 0.0177 (8) | −0.0002 (7) | 0.0020 (7) | 0.0016 (7) |
O3_2 | 0.0161 (8) | 0.0189 (9) | 0.0194 (8) | 0.0025 (7) | 0.0034 (7) | 0.0004 (7) |
O4_2 | 0.0134 (8) | 0.0189 (9) | 0.0203 (8) | −0.0018 (7) | 0.0021 (7) | −0.0024 (7) |
O5_2 | 0.0160 (9) | 0.0181 (9) | 0.0187 (8) | −0.0006 (7) | 0.0076 (7) | 0.0010 (7) |
Ni2_2 | 0.00941 (14) | 0.01073 (15) | 0.00942 (13) | 0.00003 (12) | 0.00296 (10) | 0.00057 (12) |
O6_2 | 0.0090 (7) | 0.0162 (8) | 0.0198 (8) | 0.0015 (8) | 0.0063 (6) | 0.0057 (8) |
O7_2 | 0.0094 (7) | 0.0152 (8) | 0.0124 (7) | 0.0001 (7) | 0.0031 (6) | −0.0025 (7) |
O8_2 | 0.0118 (8) | 0.0203 (9) | 0.0126 (8) | 0.0000 (7) | 0.0029 (7) | 0.0060 (7) |
O9_2 | 0.0201 (9) | 0.0122 (8) | 0.0130 (8) | 0.0007 (7) | 0.0057 (7) | 0.0008 (7) |
O10_2 | 0.0155 (8) | 0.0129 (8) | 0.0127 (8) | −0.0009 (7) | 0.0029 (6) | 0.0006 (7) |
O11_2 | 0.0207 (9) | 0.0132 (8) | 0.0127 (8) | −0.0032 (7) | 0.0058 (7) | −0.0010 (7) |
N1_2 | 0.0148 (10) | 0.0196 (11) | 0.0130 (9) | −0.0025 (8) | 0.0018 (8) | 0.0004 (8) |
O12_2 | 0.0196 (9) | 0.0175 (9) | 0.0171 (8) | −0.0003 (7) | 0.0046 (7) | −0.0006 (7) |
O13_2 | 0.0397 (11) | 0.0195 (9) | 0.0140 (8) | 0.0002 (8) | 0.0120 (8) | −0.0007 (7) |
O14_2 | 0.0576 (14) | 0.0234 (10) | 0.0186 (9) | −0.0153 (10) | 0.0172 (9) | −0.0021 (8) |
N2_2 | 0.0200 (10) | 0.0121 (10) | 0.0177 (10) | 0.0013 (8) | 0.0065 (8) | 0.0020 (8) |
O15_2 | 0.0236 (9) | 0.0184 (9) | 0.0149 (8) | 0.0016 (7) | 0.0094 (7) | 0.0016 (7) |
O16_2 | 0.0299 (10) | 0.0158 (9) | 0.0181 (8) | −0.0076 (7) | 0.0110 (7) | 0.0004 (7) |
O17_2 | 0.0373 (11) | 0.0210 (10) | 0.0202 (9) | −0.0143 (9) | 0.0043 (8) | −0.0020 (8) |
O18_2 | 0.0592 (14) | 0.0280 (11) | 0.0218 (10) | −0.0090 (10) | 0.0141 (10) | −0.0084 (9) |
Geometric parameters (Å, º) top
C1_1—O1_1 | 1.422 (3) | O18'_1—H18D_1 | 0.98 (3) |
C1_1—C2_1 | 1.509 (4) | C1_2—O1_2 | 1.427 (3) |
C1_1—H1A_1 | 0.9900 | C1_2—C2_2 | 1.503 (3) |
C1_1—H1B_1 | 0.9900 | C1_2—H1A_2 | 0.9900 |
C2_1—O2_1 | 1.433 (3) | C1_2—H1B_2 | 0.9900 |
C2_1—H2A_1 | 0.9900 | C2_2—O2_2 | 1.426 (3) |
C2_1—H2B_1 | 0.9900 | C2_2—H2A_2 | 0.9900 |
C3_1—O2_1 | 1.435 (3) | C2_2—H2B_2 | 0.9900 |
C3_1—C4_1 | 1.500 (3) | C3_2—O2_2 | 1.434 (3) |
C3_1—H3A_1 | 0.9900 | C3_2—C4_2 | 1.513 (3) |
C3_1—H3B_1 | 0.9900 | C3_2—H3A_2 | 0.9900 |
C4_1—O3_1 | 1.426 (3) | C3_2—H3B_2 | 0.9900 |
C4_1—H4A_1 | 0.9900 | C4_2—O3_2 | 1.422 (3) |
C4_1—H4B_1 | 0.9900 | C4_2—H4A_2 | 0.9900 |
C5_1—O3_1 | 1.428 (3) | C4_2—H4B_2 | 0.9900 |
C5_1—C6_1 | 1.500 (3) | C5_2—O3_2 | 1.433 (3) |
C5_1—H5A_1 | 0.9900 | C5_2—C6_2 | 1.493 (3) |
C5_1—H5B_1 | 0.9900 | C5_2—H5A_2 | 0.9900 |
C6_1—O4_1 | 1.434 (3) | C5_2—H5B_2 | 0.9900 |
C6_1—H6A_1 | 0.9900 | C6_2—O4_2 | 1.426 (3) |
C6_1—H6B_1 | 0.9900 | C6_2—H6A_2 | 0.9900 |
C7_1—O4_1 | 1.427 (3) | C6_2—H6B_2 | 0.9900 |
C7_1—C8_1 | 1.492 (3) | C7_2—O4_2 | 1.435 (3) |
C7_1—H7A_1 | 0.9900 | C7_2—C8_2 | 1.498 (3) |
C7_1—H7B_1 | 0.9900 | C7_2—H7A_2 | 0.9900 |
C8_1—O5_1 | 1.430 (3) | C7_2—H7B_2 | 0.9900 |
C8_1—H8A_1 | 0.9900 | C8_2—O5_2 | 1.431 (3) |
C8_1—H8B_1 | 0.9900 | C8_2—H8A_2 | 0.9900 |
C9_1—O5_1 | 1.424 (3) | C8_2—H8B_2 | 0.9900 |
C9_1—C10_1 | 1.496 (3) | C9_2—O5_2 | 1.433 (3) |
C9_1—H9A_1 | 0.9900 | C9_2—C10_2 | 1.504 (3) |
C9_1—H9B_1 | 0.9900 | C9_2—H9A_2 | 0.9900 |
C10_1—O1_1 | 1.433 (3) | C9_2—H9B_2 | 0.9900 |
C10_1—H10A_1 | 0.9900 | C10_2—O1_2 | 1.428 (3) |
C10_1—H10B_1 | 0.9900 | C10_2—H10A_2 | 0.9900 |
Ni1_1—O7_1 | 2.0416 (15) | C10_2—H10B_2 | 0.9900 |
Ni1_1—O6_1 | 2.0436 (14) | Ni2_2—O7_2 | 2.0355 (14) |
Ni1_1—O8_1 | 2.0440 (15) | Ni2_2—O11_2 | 2.0459 (16) |
Ni1_1—O11_1 | 2.0529 (16) | Ni2_2—O6_2 | 2.0479 (14) |
Ni1_1—O10_1 | 2.0613 (15) | Ni2_2—O8_2 | 2.0515 (15) |
Ni1_1—O9_1 | 2.0707 (16) | Ni2_2—O9_2 | 2.0538 (16) |
O6_1—H6C_1 | 0.831 (9) | Ni2_2—O10_2 | 2.0660 (15) |
O6_1—H6D_1 | 0.838 (9) | O6_2—H6C_2 | 0.832 (9) |
O7_1—H7C_1 | 0.833 (9) | O6_2—H6D_2 | 0.827 (9) |
O7_1—H7D_1 | 0.839 (9) | O7_2—H7C_2 | 0.843 (9) |
O8_1—H8C_1 | 0.828 (9) | O7_2—H7D_2 | 0.847 (9) |
O8_1—H8D_1 | 0.840 (9) | O8_2—H8C_2 | 0.832 (9) |
O9_1—H9C_1 | 0.830 (9) | O8_2—H8D_2 | 0.836 (9) |
O9_1—H9D_1 | 0.842 (9) | O9_2—H9C_2 | 0.832 (9) |
O10_1—H10C_1 | 0.848 (9) | O9_2—H9D_2 | 0.830 (9) |
O10_1—H10D_1 | 0.852 (9) | O10_2—H10C_2 | 0.848 (9) |
O11_1—H11C_1 | 0.829 (9) | O10_2—H10D_2 | 0.842 (9) |
O11_1—H11D_1 | 0.835 (9) | O11_2—H11C_2 | 0.842 (9) |
N1_1—O14_1 | 1.243 (2) | O11_2—H11D_2 | 0.841 (9) |
N1_1—O12_1 | 1.250 (2) | N1_2—O14_2 | 1.240 (2) |
N1_1—O13_1 | 1.256 (2) | N1_2—O13_2 | 1.248 (2) |
N2_1—O16_1 | 1.251 (2) | N1_2—O12_2 | 1.256 (3) |
N2_1—O15_1 | 1.251 (2) | N2_2—O15_2 | 1.247 (2) |
N2_1—O17_1 | 1.255 (3) | N2_2—O16_2 | 1.253 (2) |
O18_1—H18C_1 | 0.840 (10) | N2_2—O17_2 | 1.257 (3) |
O18_1—H18D_1 | 0.838 (10) | O18_2—H18C_2 | 0.858 (10) |
O18'_1—H18C_1 | 0.84 (3) | O18_2—H18D_2 | 0.845 (10) |
| | | |
O1_1—C1_1—C2_1 | 108.12 (19) | O1_2—C1_2—C2_2 | 108.21 (19) |
O1_1—C1_1—H1A_1 | 110.1 | O1_2—C1_2—H1A_2 | 110.1 |
C2_1—C1_1—H1A_1 | 110.1 | C2_2—C1_2—H1A_2 | 110.1 |
O1_1—C1_1—H1B_1 | 110.1 | O1_2—C1_2—H1B_2 | 110.1 |
C2_1—C1_1—H1B_1 | 110.1 | C2_2—C1_2—H1B_2 | 110.1 |
H1A_1—C1_1—H1B_1 | 108.4 | H1A_2—C1_2—H1B_2 | 108.4 |
O2_1—C2_1—C1_1 | 109.68 (19) | O2_2—C2_2—C1_2 | 109.17 (19) |
O2_1—C2_1—H2A_1 | 109.7 | O2_2—C2_2—H2A_2 | 109.8 |
C1_1—C2_1—H2A_1 | 109.7 | C1_2—C2_2—H2A_2 | 109.8 |
O2_1—C2_1—H2B_1 | 109.7 | O2_2—C2_2—H2B_2 | 109.8 |
C1_1—C2_1—H2B_1 | 109.7 | C1_2—C2_2—H2B_2 | 109.8 |
H2A_1—C2_1—H2B_1 | 108.2 | H2A_2—C2_2—H2B_2 | 108.3 |
O2_1—C3_1—C4_1 | 112.28 (19) | O2_2—C3_2—C4_2 | 111.85 (19) |
O2_1—C3_1—H3A_1 | 109.1 | O2_2—C3_2—H3A_2 | 109.2 |
C4_1—C3_1—H3A_1 | 109.1 | C4_2—C3_2—H3A_2 | 109.2 |
O2_1—C3_1—H3B_1 | 109.1 | O2_2—C3_2—H3B_2 | 109.2 |
C4_1—C3_1—H3B_1 | 109.1 | C4_2—C3_2—H3B_2 | 109.2 |
H3A_1—C3_1—H3B_1 | 107.9 | H3A_2—C3_2—H3B_2 | 107.9 |
O3_1—C4_1—C3_1 | 108.13 (19) | O3_2—C4_2—C3_2 | 107.79 (19) |
O3_1—C4_1—H4A_1 | 110.1 | O3_2—C4_2—H4A_2 | 110.1 |
C3_1—C4_1—H4A_1 | 110.1 | C3_2—C4_2—H4A_2 | 110.1 |
O3_1—C4_1—H4B_1 | 110.1 | O3_2—C4_2—H4B_2 | 110.1 |
C3_1—C4_1—H4B_1 | 110.1 | C3_2—C4_2—H4B_2 | 110.1 |
H4A_1—C4_1—H4B_1 | 108.4 | H4A_2—C4_2—H4B_2 | 108.5 |
O3_1—C5_1—C6_1 | 108.8 (2) | O3_2—C5_2—C6_2 | 108.8 (2) |
O3_1—C5_1—H5A_1 | 109.9 | O3_2—C5_2—H5A_2 | 109.9 |
C6_1—C5_1—H5A_1 | 109.9 | C6_2—C5_2—H5A_2 | 109.9 |
O3_1—C5_1—H5B_1 | 109.9 | O3_2—C5_2—H5B_2 | 109.9 |
C6_1—C5_1—H5B_1 | 109.9 | C6_2—C5_2—H5B_2 | 109.9 |
H5A_1—C5_1—H5B_1 | 108.3 | H5A_2—C5_2—H5B_2 | 108.3 |
O4_1—C6_1—C5_1 | 108.09 (19) | O4_2—C6_2—C5_2 | 108.26 (19) |
O4_1—C6_1—H6A_1 | 110.1 | O4_2—C6_2—H6A_2 | 110.0 |
C5_1—C6_1—H6A_1 | 110.1 | C5_2—C6_2—H6A_2 | 110.0 |
O4_1—C6_1—H6B_1 | 110.1 | O4_2—C6_2—H6B_2 | 110.0 |
C5_1—C6_1—H6B_1 | 110.1 | C5_2—C6_2—H6B_2 | 110.0 |
H6A_1—C6_1—H6B_1 | 108.4 | H6A_2—C6_2—H6B_2 | 108.4 |
O4_1—C7_1—C8_1 | 108.04 (19) | O4_2—C7_2—C8_2 | 108.00 (18) |
O4_1—C7_1—H7A_1 | 110.1 | O4_2—C7_2—H7A_2 | 110.1 |
C8_1—C7_1—H7A_1 | 110.1 | C8_2—C7_2—H7A_2 | 110.1 |
O4_1—C7_1—H7B_1 | 110.1 | O4_2—C7_2—H7B_2 | 110.1 |
C8_1—C7_1—H7B_1 | 110.1 | C8_2—C7_2—H7B_2 | 110.1 |
H7A_1—C7_1—H7B_1 | 108.4 | H7A_2—C7_2—H7B_2 | 108.4 |
O5_1—C8_1—C7_1 | 108.58 (19) | O5_2—C8_2—C7_2 | 106.59 (18) |
O5_1—C8_1—H8A_1 | 110.0 | O5_2—C8_2—H8A_2 | 110.4 |
C7_1—C8_1—H8A_1 | 110.0 | C7_2—C8_2—H8A_2 | 110.4 |
O5_1—C8_1—H8B_1 | 110.0 | O5_2—C8_2—H8B_2 | 110.4 |
C7_1—C8_1—H8B_1 | 110.0 | C7_2—C8_2—H8B_2 | 110.4 |
H8A_1—C8_1—H8B_1 | 108.4 | H8A_2—C8_2—H8B_2 | 108.6 |
O5_1—C9_1—C10_1 | 107.74 (19) | O5_2—C9_2—C10_2 | 107.94 (19) |
O5_1—C9_1—H9A_1 | 110.2 | O5_2—C9_2—H9A_2 | 110.1 |
C10_1—C9_1—H9A_1 | 110.2 | C10_2—C9_2—H9A_2 | 110.1 |
O5_1—C9_1—H9B_1 | 110.2 | O5_2—C9_2—H9B_2 | 110.1 |
C10_1—C9_1—H9B_1 | 110.2 | C10_2—C9_2—H9B_2 | 110.1 |
H9A_1—C9_1—H9B_1 | 108.5 | H9A_2—C9_2—H9B_2 | 108.4 |
O1_1—C10_1—C9_1 | 108.2 (2) | O1_2—C10_2—C9_2 | 107.52 (19) |
O1_1—C10_1—H10A_1 | 110.1 | O1_2—C10_2—H10A_2 | 110.2 |
C9_1—C10_1—H10A_1 | 110.1 | C9_2—C10_2—H10A_2 | 110.2 |
O1_1—C10_1—H10B_1 | 110.1 | O1_2—C10_2—H10B_2 | 110.2 |
C9_1—C10_1—H10B_1 | 110.1 | C9_2—C10_2—H10B_2 | 110.2 |
H10A_1—C10_1—H10B_1 | 108.4 | H10A_2—C10_2—H10B_2 | 108.5 |
C1_1—O1_1—C10_1 | 113.51 (19) | C1_2—O1_2—C10_2 | 112.88 (17) |
C2_1—O2_1—C3_1 | 114.08 (18) | C2_2—O2_2—C3_2 | 112.93 (18) |
C4_1—O3_1—C5_1 | 112.01 (18) | C4_2—O3_2—C5_2 | 112.77 (18) |
C7_1—O4_1—C6_1 | 114.36 (18) | C6_2—O4_2—C7_2 | 115.25 (17) |
C9_1—O5_1—C8_1 | 114.37 (18) | C8_2—O5_2—C9_2 | 114.63 (17) |
O7_1—Ni1_1—O6_1 | 173.47 (8) | O7_2—Ni2_2—O11_2 | 90.16 (7) |
O7_1—Ni1_1—O8_1 | 88.48 (6) | O7_2—Ni2_2—O6_2 | 174.76 (8) |
O6_1—Ni1_1—O8_1 | 87.50 (6) | O11_2—Ni2_2—O6_2 | 93.57 (7) |
O7_1—Ni1_1—O11_1 | 90.35 (7) | O7_2—Ni2_2—O8_2 | 89.39 (6) |
O6_1—Ni1_1—O11_1 | 94.72 (7) | O11_2—Ni2_2—O8_2 | 90.60 (6) |
O8_1—Ni1_1—O11_1 | 88.92 (7) | O6_2—Ni2_2—O8_2 | 86.90 (6) |
O7_1—Ni1_1—O10_1 | 93.11 (6) | O7_2—Ni2_2—O9_2 | 85.78 (7) |
O6_1—Ni1_1—O10_1 | 91.22 (6) | O11_2—Ni2_2—O9_2 | 173.39 (6) |
O8_1—Ni1_1—O10_1 | 176.17 (7) | O6_2—Ni2_2—O9_2 | 90.83 (7) |
O11_1—Ni1_1—O10_1 | 87.59 (6) | O8_2—Ni2_2—O9_2 | 94.56 (6) |
O7_1—Ni1_1—O9_1 | 85.65 (6) | O7_2—Ni2_2—O10_2 | 92.51 (6) |
O6_1—Ni1_1—O9_1 | 89.54 (7) | O11_2—Ni2_2—O10_2 | 87.93 (6) |
O8_1—Ni1_1—O9_1 | 94.66 (6) | O6_2—Ni2_2—O10_2 | 91.30 (6) |
O11_1—Ni1_1—O9_1 | 174.55 (7) | O8_2—Ni2_2—O10_2 | 177.61 (6) |
O10_1—Ni1_1—O9_1 | 88.94 (6) | O9_2—Ni2_2—O10_2 | 87.04 (6) |
Ni1_1—O6_1—H6C_1 | 123.2 (16) | Ni2_2—O6_2—H6C_2 | 121.4 (16) |
Ni1_1—O6_1—H6D_1 | 131.2 (15) | Ni2_2—O6_2—H6D_2 | 132.6 (16) |
H6C_1—O6_1—H6D_1 | 105.0 (14) | H6C_2—O6_2—H6D_2 | 105.6 (14) |
Ni1_1—O7_1—H7C_1 | 115.5 (15) | Ni2_2—O7_2—H7C_2 | 115.9 (15) |
Ni1_1—O7_1—H7D_1 | 124.2 (16) | Ni2_2—O7_2—H7D_2 | 123.9 (16) |
H7C_1—O7_1—H7D_1 | 104.3 (14) | H7C_2—O7_2—H7D_2 | 101.6 (13) |
Ni1_1—O8_1—H8C_1 | 117.1 (16) | Ni2_2—O8_2—H8C_2 | 115.2 (16) |
Ni1_1—O8_1—H8D_1 | 130.0 (16) | Ni2_2—O8_2—H8D_2 | 122.8 (16) |
H8C_1—O8_1—H8D_1 | 105.3 (14) | H8C_2—O8_2—H8D_2 | 104.8 (14) |
Ni1_1—O9_1—H9C_1 | 110.8 (18) | Ni2_2—O9_2—H9C_2 | 113.5 (17) |
Ni1_1—O9_1—H9D_1 | 119.4 (18) | Ni2_2—O9_2—H9D_2 | 123.4 (17) |
H9C_1—O9_1—H9D_1 | 104.4 (14) | H9C_2—O9_2—H9D_2 | 106.2 (14) |
Ni1_1—O10_1—H10C_1 | 116.2 (16) | Ni2_2—O10_2—H10C_2 | 111.2 (16) |
Ni1_1—O10_1—H10D_1 | 123.1 (16) | Ni2_2—O10_2—H10D_2 | 116.8 (17) |
H10C_1—O10_1—H10D_1 | 101.5 (13) | H10C_2—O10_2—H10D_2 | 102.6 (13) |
Ni1_1—O11_1—H11C_1 | 109.0 (17) | Ni2_2—O11_2—H11C_2 | 112.8 (17) |
Ni1_1—O11_1—H11D_1 | 123.9 (18) | Ni2_2—O11_2—H11D_2 | 122.6 (17) |
H11C_1—O11_1—H11D_1 | 105.8 (14) | H11C_2—O11_2—H11D_2 | 103.5 (14) |
O14_1—N1_1—O12_1 | 120.75 (19) | O14_2—N1_2—O13_2 | 121.0 (2) |
O14_1—N1_1—O13_1 | 120.27 (19) | O14_2—N1_2—O12_2 | 119.83 (19) |
O12_1—N1_1—O13_1 | 118.98 (18) | O13_2—N1_2—O12_2 | 119.21 (19) |
O16_1—N2_1—O15_1 | 120.01 (19) | O15_2—N2_2—O16_2 | 119.90 (18) |
O16_1—N2_1—O17_1 | 119.40 (19) | O15_2—N2_2—O17_2 | 121.22 (19) |
O15_1—N2_1—O17_1 | 120.59 (19) | O16_2—N2_2—O17_2 | 118.88 (18) |
H18C_1—O18_1—H18D_1 | 103.6 (15) | H18C_2—O18_2—H18D_2 | 101.3 (14) |
H18C_1—O18'_1—H18D_1 | 93 (3) | | |
| | | |
O1_1—C1_1—C2_1—O2_1 | 76.8 (2) | O1_2—C1_2—C2_2—O2_2 | 78.1 (2) |
O2_1—C3_1—C4_1—O3_1 | 58.0 (3) | O2_2—C3_2—C4_2—O3_2 | 55.9 (3) |
O3_1—C5_1—C6_1—O4_1 | −71.5 (2) | O3_2—C5_2—C6_2—O4_2 | −73.7 (2) |
O4_1—C7_1—C8_1—O5_1 | 66.3 (2) | O4_2—C7_2—C8_2—O5_2 | 68.9 (2) |
O5_1—C9_1—C10_1—O1_1 | −61.5 (3) | O5_2—C9_2—C10_2—O1_2 | −61.4 (2) |
C2_1—C1_1—O1_1—C10_1 | −171.00 (19) | C2_2—C1_2—O1_2—C10_2 | −166.98 (19) |
C9_1—C10_1—O1_1—C1_1 | 175.4 (2) | C9_2—C10_2—O1_2—C1_2 | 179.02 (19) |
C1_1—C2_1—O2_1—C3_1 | −166.25 (18) | C1_2—C2_2—O2_2—C3_2 | −167.92 (19) |
C4_1—C3_1—O2_1—C2_1 | 81.7 (2) | C4_2—C3_2—O2_2—C2_2 | 80.9 (2) |
C3_1—C4_1—O3_1—C5_1 | 174.5 (2) | C3_2—C4_2—O3_2—C5_2 | 171.76 (19) |
C6_1—C5_1—O3_1—C4_1 | 164.26 (19) | C6_2—C5_2—O3_2—C4_2 | 164.72 (19) |
C8_1—C7_1—O4_1—C6_1 | −170.02 (18) | C5_2—C6_2—O4_2—C7_2 | 163.88 (18) |
C5_1—C6_1—O4_1—C7_1 | 161.47 (19) | C8_2—C7_2—O4_2—C6_2 | −164.98 (19) |
C10_1—C9_1—O5_1—C8_1 | 167.88 (19) | C7_2—C8_2—O5_2—C9_2 | −164.03 (19) |
C7_1—C8_1—O5_1—C9_1 | −156.52 (19) | C10_2—C9_2—O5_2—C8_2 | 165.29 (19) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O6_1—H6C_1···O3_1 | 0.83 (1) | 2.05 (1) | 2.876 (2) | 173 (3) |
O6_1—H6D_1···O5_1 | 0.84 (1) | 1.90 (1) | 2.730 (2) | 170 (3) |
O7_1—H7C_1···O4_2 | 0.83 (1) | 1.93 (1) | 2.757 (2) | 176 (3) |
O7_1—H7D_1···O1_2 | 0.84 (1) | 1.93 (1) | 2.762 (2) | 171 (2) |
O8_1—H8C_1···O2_1 | 0.83 (1) | 2.02 (1) | 2.841 (2) | 169 (2) |
O8_1—H8D_1···O13_2i | 0.84 (1) | 2.00 (1) | 2.832 (2) | 174 (3) |
O9_1—H9C_1···O16_1ii | 0.83 (1) | 1.94 (1) | 2.763 (2) | 174 (3) |
O9_1—H9D_1···O14_1 | 0.84 (1) | 2.03 (1) | 2.860 (2) | 169 (2) |
O10_1—H10C_1···O12_1 | 0.85 (1) | 1.91 (1) | 2.742 (2) | 167 (2) |
O10_1—H10D_1···O17_1 | 0.85 (1) | 1.92 (1) | 2.766 (2) | 174 (2) |
O11_1—H11C_1···O15_1 | 0.83 (1) | 1.99 (1) | 2.782 (2) | 161 (3) |
O11_1—H11D_1···O18_1 | 0.84 (1) | 1.87 (1) | 2.703 (3) | 177 (2) |
O6_2—H6C_2···O3_2 | 0.83 (1) | 2.01 (1) | 2.828 (2) | 167 (3) |
O6_2—H6D_2···O5_2 | 0.83 (1) | 1.92 (1) | 2.746 (2) | 179 (3) |
O7_2—H7C_2···O4_1iii | 0.84 (1) | 1.94 (1) | 2.772 (2) | 171 (2) |
O7_2—H7D_2···O1_1iii | 0.85 (1) | 1.90 (1) | 2.740 (2) | 170 (2) |
O8_2—H8C_2···O2_2 | 0.83 (1) | 1.99 (1) | 2.821 (2) | 177 (3) |
O8_2—H8D_2···O13_1iv | 0.84 (1) | 2.03 (1) | 2.840 (2) | 163 (2) |
O9_2—H9C_2···O16_2v | 0.83 (1) | 1.89 (1) | 2.712 (2) | 172 (3) |
O9_2—H9D_2···O14_2 | 0.83 (1) | 2.00 (1) | 2.819 (2) | 170 (2) |
O10_2—H10C_2···O12_2 | 0.85 (1) | 1.92 (1) | 2.742 (2) | 165 (2) |
O10_2—H10D_2···O17_2 | 0.84 (1) | 1.90 (1) | 2.722 (2) | 167 (2) |
O11_2—H11C_2···O15_2 | 0.84 (1) | 1.93 (1) | 2.764 (2) | 170 (3) |
O11_2—H11D_2···O18_2 | 0.84 (1) | 1.86 (1) | 2.697 (2) | 177 (3) |
O18_2—H18D_2···O13_2vi | 0.85 (1) | 2.09 (1) | 2.930 (3) | 179 (4) |
Symmetry codes: (i) x−1/2, y, z−1/2; (ii) −x+1/2, y+1/2, −z+1/2; (iii) x+1, y, z; (iv) x+1/2, y, z−1/2; (v) −x+3/2, y+1/2, −z+1/2; (vi) −x+3/2, y−1/2, −z+1/2. |
Crystal data top
C10H20O5·H12NiO62+·2(NO3−)·H2O | Z = 6 |
Mr = 529.10 | F(000) = 1680 |
Triclinic, P1 | Dx = 1.564 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 16.036 (1) Å | Cell parameters from 11233 reflections |
b = 24.765 (2) Å | θ = 1.0–27.5° |
c = 10.163 (1) Å | µ = 0.95 mm−1 |
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 tube | 8504 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.000 |
Detector resolution: 18 pixels mm-1 | θmax = 27.5°, θmin = 1.5° |
ω scans at fixed χ = 55° | h = −20→20 |
Absorption correction: multi-scan Scalepack (Otwinowski & Minor, 2006) | k = 0→32 |
Tmin = 0.833, Tmax = 0.911 | l = −13→13 |
15437 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.064 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.159 | H 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 parameters | Δρmax = 2.08 e Å−3 |
71 restraints | Δρmin = −0.74 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C1_1 | 0.2790 (4) | 0.2665 (2) | 0.2989 (6) | 0.0313 (12) | |
H1A_1 | 0.2187 | 0.2567 | 0.2923 | 0.038* | |
H1B_1 | 0.2973 | 0.2401 | 0.2428 | 0.038* | |
C2_1 | 0.2581 (4) | 0.3233 (2) | 0.2257 (6) | 0.0302 (12) | |
H2A_1 | 0.3211 | 0.3359 | 0.2504 | 0.036* | |
H2B_1 | 0.2131 | 0.3239 | 0.1105 | 0.036* | |
C3_1 | 0.2076 (4) | 0.4152 (2) | 0.2534 (6) | 0.0311 (12) | |
H3A_1 | 0.1541 | 0.4359 | 0.2613 | 0.037* | |
H3B_1 | 0.1896 | 0.4211 | 0.1443 | 0.037* | |
C4_1 | 0.3031 (4) | 0.4368 (2) | 0.3603 (6) | 0.0307 (13) | |
H4A_1 | 0.3564 | 0.4182 | 0.3484 | 0.037* | |
H4B_1 | 0.2954 | 0.4763 | 0.3335 | 0.037* | |
C5_1 | 0.4170 (4) | 0.45132 (19) | 0.6273 (6) | 0.0278 (12) | |
H5A_1 | 0.4000 | 0.4913 | 0.6217 | 0.033* | |
H5B_1 | 0.4682 | 0.4440 | 0.6010 | 0.033* | |
C6_1 | 0.4572 (4) | 0.42710 (18) | 0.7893 (6) | 0.0279 (12) | |
H6A_1 | 0.5080 | 0.4484 | 0.8679 | 0.033* | |
H6B_1 | 0.4027 | 0.4276 | 0.8082 | 0.033* | |
C7_1 | 0.5212 (4) | 0.33931 (19) | 0.9340 (6) | 0.0272 (12) | |
H7A_1 | 0.4634 | 0.3449 | 0.9454 | 0.033* | |
H7B_1 | 0.5803 | 0.3494 | 1.0306 | 0.033* | |
C8_1 | 0.5404 (4) | 0.28075 (19) | 0.9077 (6) | 0.0282 (12) | |
H8A_1 | 0.5938 | 0.2761 | 0.8858 | 0.034* | |
H8B_1 | 0.5623 | 0.2571 | 1.0026 | 0.034* | |
C9_1 | 0.4647 (4) | 0.21859 (19) | 0.7091 (6) | 0.0281 (12) | |
H9A_1 | 0.4774 | 0.1854 | 0.7753 | 0.034* | |
H9B_1 | 0.5229 | 0.2198 | 0.7002 | 0.034* | |
C10_1 | 0.3723 (4) | 0.21719 (18) | 0.5500 (6) | 0.0261 (12) | |
H10A_1 | 0.3796 | 0.1842 | 0.5006 | 0.031* | |
H10B_1 | 0.3138 | 0.2164 | 0.5584 | 0.031* | |
O1_1 | 0.3591 (2) | 0.26482 (12) | 0.4585 (4) | 0.0266 (8) | |
O2_1 | 0.2120 (2) | 0.35837 (13) | 0.2873 (4) | 0.0295 (8) | |
O3_1 | 0.3299 (2) | 0.42777 (12) | 0.5185 (4) | 0.0245 (8) | |
O4_1 | 0.5012 (2) | 0.37206 (12) | 0.8018 (4) | 0.0252 (8) | |
O5_1 | 0.4504 (2) | 0.26596 (12) | 0.7782 (4) | 0.0227 (7) | |
Ni1_1 | 0.15027 (4) | 0.34278 (2) | 0.62164 (7) | 0.02277 (16) | |
O6_1 | 0.2848 (2) | 0.34488 (13) | 0.6480 (4) | 0.0263 (8) | |
H6C_1 | 0.291 (3) | 0.3683 (14) | 0.595 (5) | 0.039* | |
H6D_1 | 0.329 (3) | 0.3193 (13) | 0.671 (6) | 0.039* | |
O7_1 | 0.0096 (2) | 0.34550 (13) | 0.5774 (4) | 0.0249 (8) | |
H7C_1 | −0.022 (3) | 0.3197 (15) | 0.537 (5) | 0.037* | |
H7D_1 | −0.012 (3) | 0.3590 (17) | 0.630 (5) | 0.037* | |
O8_1 | 0.0817 (3) | 0.34957 (18) | 0.3832 (4) | 0.0432 (10) | |
H8C_1 | 0.119 (3) | 0.348 (2) | 0.348 (6) | 0.065* | |
H8D_1 | 0.033 (3) | 0.372 (2) | 0.321 (6) | 0.065* | |
O9_1 | 0.1420 (4) | 0.42601 (16) | 0.6349 (6) | 0.0561 (13) | |
H9C_1 | 0.089 (3) | 0.447 (2) | 0.582 (6) | 0.084* | |
H9D_1 | 0.160 (5) | 0.431 (3) | 0.729 (3) | 0.084* | |
O10_1 | 0.2212 (2) | 0.33229 (15) | 0.8613 (4) | 0.0303 (8) | |
H10C_1 | 0.254 (3) | 0.3576 (12) | 0.908 (6) | 0.045* | |
H10D_1 | 0.261 (3) | 0.3035 (11) | 0.906 (6) | 0.045* | |
O11_1 | 0.1580 (2) | 0.26040 (13) | 0.6186 (4) | 0.0261 (8) | |
H11C_1 | 0.134 (3) | 0.2432 (17) | 0.538 (3) | 0.039* | |
H11D_1 | 0.206 (3) | 0.2382 (16) | 0.688 (4) | 0.039* | |
N1_1 | 0.3843 (3) | 0.43690 (18) | 1.0881 (5) | 0.0305 (10) | |
O12_1 | 0.3816 (3) | 0.38606 (14) | 1.0931 (4) | 0.0342 (9) | |
O13_1 | 0.4425 (3) | 0.45868 (14) | 1.2100 (4) | 0.0344 (9) | |
O14_1 | 0.3269 (3) | 0.46528 (16) | 0.9633 (4) | 0.0472 (11) | |
N2_1 | 0.3915 (3) | 0.20732 (17) | 0.9679 (5) | 0.0293 (10) | |
O15_1 | 0.3209 (3) | 0.19180 (13) | 0.8469 (4) | 0.0286 (8) | |
O16_1 | 0.4752 (3) | 0.17882 (13) | 1.0371 (4) | 0.0329 (9) | |
O17_1 | 0.3794 (3) | 0.25089 (14) | 1.0224 (4) | 0.0356 (9) | |
N3_1 | −0.0710 (8) | 0.4708 (4) | 0.1906 (13) | 0.0286 (14) | 0.529 (6) |
O19_1 | −0.0550 (7) | 0.4235 (3) | 0.1597 (11) | 0.0384 (17) | 0.529 (6) |
O20_1 | −0.0306 (18) | 0.4818 (8) | 0.3291 (12) | 0.035 (3) | 0.529 (6) |
O21_1 | −0.1278 (7) | 0.5067 (4) | 0.0813 (10) | 0.0471 (19) | 0.529 (6) |
N3'_1 | −0.0693 (9) | 0.4817 (4) | 0.1946 (14) | 0.0286 (14) | 0.471 (6) |
O19'_1 | −0.0807 (8) | 0.4482 (4) | 0.0964 (12) | 0.0384 (17) | 0.471 (6) |
O20'_1 | −0.011 (2) | 0.4677 (9) | 0.3363 (13) | 0.035 (3) | 0.471 (6) |
O21'_1 | −0.1168 (8) | 0.5289 (4) | 0.1504 (12) | 0.0471 (19) | 0.471 (6) |
O18_1 | 0.1026 (3) | 0.20811 (16) | 0.3581 (5) | 0.0451 (10) | |
H18C_1 | 0.080 (4) | 0.194 (2) | 0.406 (5) | 0.068* | |
H18D_1 | 0.056 (3) | 0.207 (3) | 0.2636 (19) | 0.068* | |
C1_2 | 0.8302 (4) | 0.2537 (2) | 0.3078 (6) | 0.0300 (12) | |
H1A_2 | 0.7683 | 0.2445 | 0.2968 | 0.036* | |
H1B_2 | 0.8530 | 0.2254 | 0.2613 | 0.036* | |
C2_2 | 0.8106 (4) | 0.3084 (2) | 0.2261 (6) | 0.0307 (12) | |
H2A_2 | 0.8740 | 0.3196 | 0.2480 | 0.037* | |
H2B_2 | 0.7656 | 0.3068 | 0.1116 | 0.037* | |
C3_2 | 0.7742 (4) | 0.4017 (2) | 0.2496 (6) | 0.0349 (13) | |
H3A_2 | 0.7452 | 0.4092 | 0.1363 | 0.042* | |
H3B_2 | 0.8454 | 0.4070 | 0.3072 | 0.042* | |
C4_2 | 0.7195 (4) | 0.4393 (2) | 0.3013 (6) | 0.0323 (13) | |
H4A_2 | 0.7247 | 0.4774 | 0.2801 | 0.039* | |
H4B_2 | 0.6479 | 0.4346 | 0.2397 | 0.039* | |
C5_2 | 0.8431 (4) | 0.45550 (19) | 0.5653 (6) | 0.0280 (12) | |
H5A_2 | 0.8236 | 0.4954 | 0.5534 | 0.034* | |
H5B_2 | 0.8936 | 0.4478 | 0.5377 | 0.034* | |
C6_2 | 0.8864 (4) | 0.43424 (19) | 0.7320 (6) | 0.0288 (12) | |
H6A_2 | 0.9333 | 0.4583 | 0.8055 | 0.035* | |
H6B_2 | 0.8324 | 0.4332 | 0.7517 | 0.035* | |
C7_2 | 0.9661 (4) | 0.35126 (19) | 0.8967 (6) | 0.0288 (12) | |
H7A_2 | 0.9067 | 0.3484 | 0.9014 | 0.035* | |
H7B_2 | 1.0131 | 0.3704 | 0.9876 | 0.035* | |
C8_2 | 1.0152 (3) | 0.2957 (2) | 0.9001 (6) | 0.0268 (12) | |
H8A_2 | 1.0744 | 0.2988 | 0.8949 | 0.032* | |
H8B_2 | 1.0374 | 0.2743 | 0.9987 | 0.032* | |
C9_2 | 0.9881 (4) | 0.22267 (19) | 0.7336 (6) | 0.0274 (12) | |
H9A_2 | 1.0017 | 0.1907 | 0.8045 | 0.033* | |
H9B_2 | 1.0520 | 0.2296 | 0.7478 | 0.033* | |
C10_2 | 0.9169 (4) | 0.21163 (19) | 0.5684 (6) | 0.0271 (12) | |
H10A_2 | 0.9426 | 0.1776 | 0.5438 | 0.033* | |
H10B_2 | 0.8516 | 0.2071 | 0.5526 | 0.033* | |
O1_2 | 0.9051 (2) | 0.25586 (13) | 0.4684 (4) | 0.0259 (8) | |
O2_2 | 0.7652 (2) | 0.34684 (13) | 0.2813 (4) | 0.0279 (8) | |
O3_2 | 0.7580 (2) | 0.42952 (13) | 0.4644 (4) | 0.0271 (8) | |
O4_2 | 0.9376 (2) | 0.38054 (13) | 0.7545 (4) | 0.0290 (8) | |
O5_2 | 0.9450 (2) | 0.26934 (12) | 0.7696 (4) | 0.0226 (7) | |
Ni2_2 | 0.62237 (4) | 0.32005 (2) | 0.54131 (7) | 0.01885 (15) | |
O6_2 | 0.7467 (2) | 0.30770 (14) | 0.5296 (4) | 0.0244 (8) | |
H6C_2 | 0.8080 (17) | 0.304 (2) | 0.603 (3) | 0.037* | |
H6D_2 | 0.749 (3) | 0.319 (2) | 0.453 (3) | 0.037* | |
O7_2 | 0.4962 (2) | 0.33451 (13) | 0.5435 (4) | 0.0213 (7) | |
H7C_2 | 0.505 (3) | 0.3432 (19) | 0.629 (3) | 0.032* | |
H7D_2 | 0.451 (3) | 0.3149 (17) | 0.510 (5) | 0.032* | |
O8_2 | 0.5373 (2) | 0.30468 (14) | 0.3082 (4) | 0.0292 (8) | |
H8C_2 | 0.498 (3) | 0.3301 (12) | 0.248 (5) | 0.044* | |
H8D_2 | 0.519 (4) | 0.2759 (10) | 0.270 (5) | 0.044* | |
O9_2 | 0.6033 (2) | 0.40150 (13) | 0.4837 (4) | 0.0253 (8) | |
H9C_2 | 0.556 (2) | 0.4151 (19) | 0.394 (3) | 0.038* | |
H9D_2 | 0.653 (2) | 0.4122 (19) | 0.492 (5) | 0.038* | |
O10_2 | 0.7059 (2) | 0.33529 (13) | 0.7716 (4) | 0.0279 (8) | |
H10C_2 | 0.749 (3) | 0.3127 (14) | 0.841 (4) | 0.042* | |
H10D_2 | 0.706 (4) | 0.3643 (11) | 0.814 (5) | 0.042* | |
O11_2 | 0.6428 (2) | 0.24089 (12) | 0.6165 (4) | 0.0238 (7) | |
H11C_2 | 0.699 (2) | 0.2215 (17) | 0.674 (4) | 0.036* | |
H11D_2 | 0.612 (3) | 0.2243 (17) | 0.536 (3) | 0.036* | |
N1_2 | 0.8786 (3) | 0.20335 (16) | 0.9464 (5) | 0.0238 (9) | |
O12_2 | 0.8294 (2) | 0.18434 (12) | 0.8163 (4) | 0.0253 (8) | |
O13_2 | 0.9631 (3) | 0.17879 (13) | 1.0491 (4) | 0.0342 (9) | |
O14_2 | 0.8467 (3) | 0.24665 (13) | 0.9771 (4) | 0.0341 (9) | |
N2_2 | 0.5444 (3) | 0.14610 (16) | 0.3622 (5) | 0.0279 (10) | |
O15_2 | 0.5035 (3) | 0.18818 (14) | 0.3853 (4) | 0.0401 (10) | |
O16_2 | 0.4926 (2) | 0.10942 (13) | 0.2896 (4) | 0.0259 (8) | |
O17_2 | 0.6350 (2) | 0.14147 (15) | 0.4125 (4) | 0.0373 (9) | |
O18_2 | 0.7175 (3) | 0.43898 (14) | 0.8631 (4) | 0.0364 (9) | |
H18C_2 | 0.7697 (19) | 0.449 (2) | 0.937 (5) | 0.055* | |
H18D_2 | 0.672 (2) | 0.4630 (16) | 0.849 (6) | 0.055* | |
C1_3 | 0.3655 (3) | 0.02904 (19) | 0.3486 (6) | 0.0249 (11) | |
H1A_3 | 0.3905 | 0.0438 | 0.4519 | 0.030* | |
H1B_3 | 0.4089 | 0.0376 | 0.3119 | 0.030* | |
C2_3 | 0.3677 (4) | −0.03137 (19) | 0.3629 (6) | 0.0267 (11) | |
H2A_3 | 0.4308 | −0.0478 | 0.4583 | 0.032* | |
H2B_3 | 0.3114 | −0.0398 | 0.3704 | 0.032* | |
C3_3 | 0.3374 (4) | −0.10797 (18) | 0.2083 (6) | 0.0280 (12) | |
H3A_3 | 0.2786 | −0.1107 | 0.2148 | 0.034* | |
H3B_3 | 0.3947 | −0.1328 | 0.2929 | 0.034* | |
C4_3 | 0.3164 (4) | −0.1238 (2) | 0.0541 (6) | 0.0286 (12) | |
H4A_3 | 0.3729 | −0.1180 | 0.0439 | 0.034* | |
H4B_3 | 0.3080 | −0.1629 | 0.0442 | 0.034* | |
C5_3 | 0.2147 (4) | −0.0882 (2) | −0.2158 (6) | 0.0305 (12) | |
H5A_3 | 0.1912 | −0.1218 | −0.2685 | 0.037* | |
H5B_3 | 0.2791 | −0.0843 | −0.2041 | 0.037* | |
C6_3 | 0.1388 (4) | −0.03938 (19) | −0.3110 (6) | 0.0281 (12) | |
H6A_3 | 0.1260 | −0.0369 | −0.4178 | 0.034* | |
H6B_3 | 0.0751 | −0.0425 | −0.3196 | 0.034* | |
C7_3 | 0.1114 (3) | 0.05682 (19) | −0.3062 (6) | 0.0244 (11) | |
H7A_3 | 0.0497 | 0.0548 | −0.3075 | 0.029* | |
H7B_3 | 0.0932 | 0.0624 | −0.4156 | 0.029* | |
C8_3 | 0.1625 (4) | 0.10310 (19) | −0.2146 (6) | 0.0246 (11) | |
H8A_3 | 0.2308 | 0.1002 | −0.1935 | 0.030* | |
H8B_3 | 0.1250 | 0.1383 | −0.2754 | 0.030* | |
C9_3 | 0.2522 (4) | 0.1225 (2) | 0.0562 (6) | 0.0267 (12) | |
H9A_3 | 0.2459 | 0.1624 | 0.0353 | 0.032* | |
H9B_3 | 0.3145 | 0.1052 | 0.0672 | 0.032* | |
C10_3 | 0.2545 (4) | 0.11071 (18) | 0.2022 (6) | 0.0256 (11) | |
H10A_3 | 0.3110 | 0.1263 | 0.2903 | 0.031* | |
H10B_3 | 0.1921 | 0.1287 | 0.1898 | 0.031* | |
O1_3 | 0.2650 (2) | 0.05326 (12) | 0.2394 (4) | 0.0261 (8) | |
O2_3 | 0.3597 (2) | −0.05312 (12) | 0.2262 (4) | 0.0246 (8) | |
O3_3 | 0.2268 (2) | −0.09107 (13) | −0.0662 (4) | 0.0275 (8) | |
O4_3 | 0.1788 (2) | 0.00773 (13) | −0.2328 (4) | 0.0268 (8) | |
O5_3 | 0.1670 (2) | 0.10086 (13) | −0.0709 (4) | 0.0239 (8) | |
Ni3_3 | 0.0000 | 0.0000 | 0.0000 | 0.0171 (2) | |
O6_3 | 0.1414 (2) | −0.01993 (13) | 0.0544 (4) | 0.0223 (7) | |
H6C_3 | 0.180 (3) | 0.0034 (15) | 0.099 (5) | 0.033* | |
H6D_3 | 0.162 (3) | −0.0369 (16) | 0.007 (5) | 0.033* | |
O8_3 | −0.0094 (2) | −0.08018 (12) | 0.0401 (4) | 0.0229 (7) | |
H8C_3 | −0.059 (2) | −0.0863 (17) | 0.042 (6) | 0.034* | |
H8D_3 | 0.008 (3) | −0.1090 (13) | 0.014 (6) | 0.034* | |
O9_3 | −0.0544 (2) | −0.00654 (13) | −0.2317 (4) | 0.0214 (7) | |
H9C_3 | −0.082 (3) | −0.0344 (10) | −0.272 (5) | 0.032* | |
H9D_3 | −0.097 (3) | 0.0195 (11) | −0.289 (5) | 0.032* | |
Ni4_3 | 0.5000 | 0.0000 | 0.0000 | 0.0182 (2) | |
O7_3 | 0.6242 (2) | −0.00758 (13) | −0.0129 (4) | 0.0236 (8) | |
H7C_3 | 0.680 (2) | −0.005 (2) | 0.069 (3) | 0.035* | |
H7D_3 | 0.622 (3) | 0.0122 (17) | −0.082 (4) | 0.035* | |
O10_3 | 0.4206 (3) | −0.02794 (15) | −0.2143 (4) | 0.0361 (9) | |
H10C_3 | 0.373 (3) | −0.0094 (18) | −0.294 (4) | 0.054* | |
H10D_3 | 0.436 (4) | −0.0549 (14) | −0.251 (5) | 0.054* | |
O11_3 | 0.4580 (2) | 0.07835 (12) | −0.1048 (4) | 0.0246 (8) | |
H11C_3 | 0.413 (3) | 0.0858 (18) | −0.199 (2) | 0.037* | |
H11D_3 | 0.461 (3) | 0.1075 (13) | −0.062 (4) | 0.037* | |
N1_3 | 0.2312 (3) | 0.07350 (16) | 0.5055 (5) | 0.0240 (9) | |
O12_3 | 0.2489 (2) | 0.02283 (13) | 0.5351 (4) | 0.0283 (8) | |
O13_3 | 0.2959 (3) | 0.10350 (14) | 0.5829 (4) | 0.0330 (9) | |
O14_3 | 0.1451 (2) | 0.09433 (13) | 0.3932 (4) | 0.0262 (8) | |
O18_3 | 0.1601 (3) | −0.09401 (13) | 0.3819 (4) | 0.0285 (8) | |
H18C_3 | 0.2216 (10) | −0.1029 (19) | 0.439 (4) | 0.043* | |
H18D_3 | 0.141 (3) | −0.1126 (18) | 0.306 (4) | 0.043* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1_1 | 0.033 (3) | 0.035 (3) | 0.028 (3) | −0.012 (2) | 0.016 (3) | −0.009 (2) |
C2_1 | 0.033 (3) | 0.039 (3) | 0.027 (3) | −0.010 (2) | 0.021 (3) | −0.008 (2) |
C3_1 | 0.028 (3) | 0.032 (3) | 0.034 (3) | 0.004 (2) | 0.019 (3) | 0.008 (2) |
C4_1 | 0.038 (3) | 0.022 (3) | 0.038 (3) | 0.002 (2) | 0.026 (3) | 0.010 (2) |
C5_1 | 0.032 (3) | 0.016 (2) | 0.041 (3) | −0.004 (2) | 0.023 (3) | −0.001 (2) |
C6_1 | 0.039 (3) | 0.016 (3) | 0.036 (3) | −0.003 (2) | 0.025 (3) | −0.009 (2) |
C7_1 | 0.023 (3) | 0.031 (3) | 0.020 (3) | −0.004 (2) | 0.007 (2) | 0.001 (2) |
C8_1 | 0.022 (3) | 0.024 (3) | 0.033 (3) | 0.000 (2) | 0.012 (3) | 0.004 (2) |
C9_1 | 0.029 (3) | 0.022 (3) | 0.036 (3) | 0.006 (2) | 0.021 (3) | 0.003 (2) |
C10_1 | 0.034 (3) | 0.018 (3) | 0.035 (3) | −0.007 (2) | 0.024 (3) | −0.007 (2) |
O1_1 | 0.0267 (19) | 0.0218 (18) | 0.030 (2) | −0.0069 (15) | 0.0140 (18) | −0.0028 (15) |
O2_1 | 0.028 (2) | 0.030 (2) | 0.034 (2) | −0.0013 (16) | 0.0191 (18) | 0.0026 (16) |
O3_1 | 0.0258 (19) | 0.0208 (18) | 0.029 (2) | 0.0014 (14) | 0.0167 (17) | 0.0041 (15) |
O4_1 | 0.0294 (19) | 0.0206 (18) | 0.032 (2) | −0.0023 (15) | 0.0213 (18) | −0.0017 (15) |
O5_1 | 0.0199 (18) | 0.0168 (17) | 0.030 (2) | 0.0034 (14) | 0.0135 (17) | 0.0003 (15) |
Ni1_1 | 0.0204 (3) | 0.0214 (3) | 0.0297 (4) | 0.0008 (3) | 0.0163 (3) | 0.0018 (3) |
O6_1 | 0.0230 (19) | 0.0214 (19) | 0.039 (2) | 0.0021 (14) | 0.0209 (18) | 0.0063 (16) |
O7_1 | 0.0204 (19) | 0.0253 (19) | 0.035 (2) | 0.0008 (15) | 0.0198 (18) | 0.0018 (16) |
O8_1 | 0.022 (2) | 0.074 (3) | 0.029 (2) | −0.0028 (19) | 0.0108 (19) | 0.017 (2) |
O9_1 | 0.062 (3) | 0.021 (2) | 0.116 (4) | 0.003 (2) | 0.070 (3) | 0.006 (3) |
O10_1 | 0.028 (2) | 0.036 (2) | 0.030 (2) | −0.0073 (16) | 0.0173 (18) | −0.0110 (18) |
O11_1 | 0.024 (2) | 0.0230 (19) | 0.027 (2) | −0.0014 (15) | 0.0115 (17) | −0.0035 (15) |
N1_1 | 0.036 (3) | 0.035 (3) | 0.030 (3) | −0.002 (2) | 0.025 (2) | 0.000 (2) |
O12_1 | 0.039 (2) | 0.024 (2) | 0.038 (2) | 0.0001 (17) | 0.020 (2) | −0.0035 (17) |
O13_1 | 0.034 (2) | 0.028 (2) | 0.037 (2) | −0.0105 (17) | 0.016 (2) | −0.0035 (18) |
O14_1 | 0.051 (3) | 0.049 (3) | 0.030 (2) | 0.017 (2) | 0.019 (2) | 0.017 (2) |
N2_1 | 0.032 (3) | 0.024 (2) | 0.036 (3) | 0.001 (2) | 0.021 (2) | 0.007 (2) |
O15_1 | 0.028 (2) | 0.0230 (19) | 0.030 (2) | −0.0054 (16) | 0.0120 (18) | −0.0012 (16) |
O16_1 | 0.029 (2) | 0.029 (2) | 0.037 (2) | 0.0072 (16) | 0.0176 (19) | 0.0098 (17) |
O17_1 | 0.038 (2) | 0.028 (2) | 0.034 (2) | 0.0025 (17) | 0.0170 (19) | −0.0016 (17) |
N3_1 | 0.022 (3) | 0.033 (4) | 0.031 (3) | −0.008 (3) | 0.014 (2) | −0.005 (3) |
O19_1 | 0.038 (4) | 0.032 (5) | 0.042 (5) | 0.007 (4) | 0.021 (4) | −0.010 (3) |
O20_1 | 0.026 (9) | 0.034 (9) | 0.030 (3) | 0.007 (5) | 0.006 (3) | 0.002 (3) |
O21_1 | 0.043 (4) | 0.040 (5) | 0.038 (5) | 0.017 (4) | 0.012 (4) | 0.014 (3) |
N3'_1 | 0.022 (3) | 0.033 (4) | 0.031 (3) | −0.008 (3) | 0.014 (2) | −0.005 (3) |
O19'_1 | 0.038 (4) | 0.032 (5) | 0.042 (5) | 0.007 (4) | 0.021 (4) | −0.010 (3) |
O20'_1 | 0.026 (9) | 0.034 (9) | 0.030 (3) | 0.007 (5) | 0.006 (3) | 0.002 (3) |
O21'_1 | 0.043 (4) | 0.040 (5) | 0.038 (5) | 0.017 (4) | 0.012 (4) | 0.014 (3) |
O18_1 | 0.055 (3) | 0.036 (2) | 0.037 (2) | −0.006 (2) | 0.020 (2) | −0.008 (2) |
C1_2 | 0.031 (3) | 0.033 (3) | 0.025 (3) | 0.000 (2) | 0.015 (3) | −0.005 (2) |
C2_2 | 0.031 (3) | 0.037 (3) | 0.027 (3) | −0.001 (2) | 0.018 (3) | −0.006 (2) |
C3_2 | 0.042 (3) | 0.037 (3) | 0.030 (3) | −0.001 (3) | 0.024 (3) | 0.010 (3) |
C4_2 | 0.031 (3) | 0.036 (3) | 0.026 (3) | 0.002 (2) | 0.015 (3) | 0.007 (2) |
C5_2 | 0.029 (3) | 0.016 (3) | 0.045 (3) | 0.001 (2) | 0.024 (3) | 0.000 (2) |
C6_2 | 0.028 (3) | 0.026 (3) | 0.036 (3) | 0.000 (2) | 0.020 (3) | −0.007 (2) |
C7_2 | 0.033 (3) | 0.027 (3) | 0.027 (3) | −0.004 (2) | 0.017 (3) | −0.004 (2) |
C8_2 | 0.021 (3) | 0.034 (3) | 0.024 (3) | −0.002 (2) | 0.011 (2) | 0.002 (2) |
C9_2 | 0.027 (3) | 0.024 (3) | 0.035 (3) | 0.004 (2) | 0.021 (3) | 0.001 (2) |
C10_2 | 0.034 (3) | 0.019 (3) | 0.033 (3) | 0.002 (2) | 0.022 (3) | −0.001 (2) |
O1_2 | 0.0283 (19) | 0.0258 (19) | 0.024 (2) | −0.0013 (15) | 0.0152 (17) | 0.0005 (15) |
O2_2 | 0.033 (2) | 0.0260 (19) | 0.027 (2) | 0.0002 (15) | 0.0177 (18) | 0.0005 (15) |
O3_2 | 0.031 (2) | 0.0227 (18) | 0.031 (2) | −0.0039 (15) | 0.0186 (18) | 0.0019 (15) |
O4_2 | 0.035 (2) | 0.0260 (19) | 0.031 (2) | −0.0013 (16) | 0.0218 (18) | 0.0008 (16) |
O5_2 | 0.0185 (18) | 0.0198 (17) | 0.0245 (19) | 0.0026 (14) | 0.0094 (16) | −0.0003 (15) |
Ni2_2 | 0.0186 (3) | 0.0166 (3) | 0.0229 (4) | 0.0010 (2) | 0.0129 (3) | 0.0004 (3) |
O6_2 | 0.0187 (18) | 0.0294 (19) | 0.026 (2) | 0.0039 (15) | 0.0143 (16) | 0.0054 (16) |
O7_2 | 0.0160 (18) | 0.0243 (19) | 0.027 (2) | −0.0036 (14) | 0.0133 (17) | −0.0055 (15) |
O8_2 | 0.030 (2) | 0.030 (2) | 0.025 (2) | 0.0002 (16) | 0.0135 (18) | −0.0049 (16) |
O9_2 | 0.0237 (19) | 0.0182 (18) | 0.033 (2) | 0.0011 (15) | 0.0152 (17) | 0.0070 (15) |
O10_2 | 0.027 (2) | 0.0207 (19) | 0.028 (2) | 0.0067 (15) | 0.0118 (18) | 0.0016 (16) |
O11_2 | 0.0255 (19) | 0.0184 (18) | 0.026 (2) | −0.0005 (14) | 0.0131 (17) | −0.0031 (15) |
N1_2 | 0.027 (2) | 0.020 (2) | 0.024 (3) | 0.0014 (19) | 0.015 (2) | 0.0003 (19) |
O12_2 | 0.0251 (19) | 0.0223 (18) | 0.026 (2) | −0.0012 (15) | 0.0124 (17) | −0.0036 (16) |
O13_2 | 0.030 (2) | 0.0252 (19) | 0.033 (2) | 0.0101 (16) | 0.0103 (19) | −0.0044 (16) |
O14_2 | 0.046 (2) | 0.024 (2) | 0.032 (2) | 0.0139 (17) | 0.025 (2) | 0.0023 (16) |
N2_2 | 0.030 (3) | 0.025 (2) | 0.027 (3) | 0.001 (2) | 0.016 (2) | −0.002 (2) |
O15_2 | 0.036 (2) | 0.031 (2) | 0.055 (3) | −0.0017 (17) | 0.027 (2) | −0.0195 (19) |
O16_2 | 0.0266 (19) | 0.0237 (18) | 0.028 (2) | −0.0083 (15) | 0.0147 (17) | −0.0041 (16) |
O17_2 | 0.017 (2) | 0.045 (2) | 0.041 (2) | −0.0058 (17) | 0.0093 (18) | −0.0058 (18) |
O18_2 | 0.047 (2) | 0.029 (2) | 0.038 (2) | −0.0062 (18) | 0.026 (2) | −0.0077 (18) |
C1_3 | 0.021 (3) | 0.030 (3) | 0.022 (3) | −0.003 (2) | 0.010 (2) | −0.001 (2) |
C2_3 | 0.029 (3) | 0.027 (3) | 0.021 (3) | −0.001 (2) | 0.011 (2) | 0.003 (2) |
C3_3 | 0.029 (3) | 0.017 (3) | 0.036 (3) | 0.004 (2) | 0.018 (3) | 0.005 (2) |
C4_3 | 0.026 (3) | 0.022 (3) | 0.041 (3) | 0.002 (2) | 0.021 (3) | 0.002 (2) |
C5_3 | 0.037 (3) | 0.028 (3) | 0.038 (3) | −0.008 (2) | 0.027 (3) | −0.010 (2) |
C6_3 | 0.028 (3) | 0.027 (3) | 0.031 (3) | −0.008 (2) | 0.015 (3) | −0.010 (2) |
C7_3 | 0.022 (3) | 0.030 (3) | 0.021 (3) | 0.007 (2) | 0.014 (2) | 0.005 (2) |
C8_3 | 0.026 (3) | 0.023 (3) | 0.030 (3) | 0.002 (2) | 0.020 (3) | 0.004 (2) |
C9_3 | 0.026 (3) | 0.028 (3) | 0.029 (3) | −0.007 (2) | 0.016 (3) | −0.004 (2) |
C10_3 | 0.031 (3) | 0.021 (3) | 0.028 (3) | −0.002 (2) | 0.018 (3) | −0.002 (2) |
O1_3 | 0.0233 (19) | 0.0209 (18) | 0.029 (2) | −0.0029 (14) | 0.0113 (17) | 0.0013 (15) |
O2_3 | 0.0288 (19) | 0.0169 (17) | 0.035 (2) | 0.0000 (14) | 0.0219 (18) | 0.0006 (15) |
O3_3 | 0.028 (2) | 0.0275 (19) | 0.031 (2) | 0.0003 (15) | 0.0199 (18) | −0.0033 (16) |
O4_3 | 0.0269 (19) | 0.0227 (18) | 0.028 (2) | −0.0014 (15) | 0.0136 (17) | −0.0028 (15) |
O5_3 | 0.0201 (18) | 0.0309 (19) | 0.0225 (19) | −0.0036 (15) | 0.0128 (16) | −0.0028 (15) |
Ni3_3 | 0.0146 (4) | 0.0162 (4) | 0.0201 (5) | 0.0018 (3) | 0.0097 (4) | 0.0000 (4) |
O6_3 | 0.0145 (18) | 0.0251 (19) | 0.031 (2) | −0.0024 (14) | 0.0146 (17) | −0.0092 (15) |
O8_3 | 0.026 (2) | 0.0155 (17) | 0.033 (2) | −0.0009 (14) | 0.0204 (18) | −0.0018 (15) |
O9_3 | 0.0204 (18) | 0.0180 (17) | 0.0221 (19) | 0.0012 (14) | 0.0098 (16) | −0.0016 (15) |
Ni4_3 | 0.0175 (5) | 0.0165 (4) | 0.0210 (5) | 0.0018 (3) | 0.0115 (4) | 0.0009 (4) |
O7_3 | 0.0194 (18) | 0.0226 (18) | 0.033 (2) | 0.0024 (15) | 0.0176 (17) | 0.0051 (16) |
O10_3 | 0.034 (2) | 0.033 (2) | 0.024 (2) | 0.0105 (17) | 0.0072 (19) | −0.0079 (17) |
O11_3 | 0.029 (2) | 0.0163 (17) | 0.028 (2) | 0.0019 (15) | 0.0157 (18) | 0.0030 (15) |
N1_3 | 0.029 (3) | 0.028 (2) | 0.020 (2) | −0.005 (2) | 0.017 (2) | −0.006 (2) |
O12_3 | 0.028 (2) | 0.0208 (19) | 0.032 (2) | 0.0005 (15) | 0.0144 (18) | 0.0022 (16) |
O13_3 | 0.031 (2) | 0.028 (2) | 0.030 (2) | −0.0113 (17) | 0.0093 (18) | −0.0040 (17) |
O14_3 | 0.0218 (19) | 0.0247 (18) | 0.024 (2) | 0.0046 (15) | 0.0084 (17) | 0.0028 (15) |
O18_3 | 0.031 (2) | 0.025 (2) | 0.027 (2) | 0.0009 (16) | 0.0146 (18) | −0.0004 (16) |
Geometric parameters (Å, º) top
C1_1—O1_1 | 1.424 (6) | C9_2—C10_2 | 1.487 (7) |
C1_1—C2_1 | 1.503 (7) | C9_2—H9A_2 | 0.9900 |
C1_1—H1A_1 | 0.9900 | C9_2—H9B_2 | 0.9900 |
C1_1—H1B_1 | 0.9900 | C10_2—O1_2 | 1.416 (5) |
C2_1—O2_1 | 1.433 (6) | C10_2—H10A_2 | 0.9900 |
C2_1—H2A_1 | 0.9900 | C10_2—H10B_2 | 0.9900 |
C2_1—H2B_1 | 0.9900 | Ni2_2—O11_2 | 2.027 (3) |
C3_1—O2_1 | 1.432 (6) | Ni2_2—O7_2 | 2.027 (3) |
C3_1—C4_1 | 1.488 (7) | Ni2_2—O9_2 | 2.040 (3) |
C3_1—H3A_1 | 0.9900 | Ni2_2—O10_2 | 2.041 (3) |
C3_1—H3B_1 | 0.9900 | Ni2_2—O6_2 | 2.051 (3) |
C4_1—O3_1 | 1.433 (6) | Ni2_2—O8_2 | 2.066 (3) |
C4_1—H4A_1 | 0.9900 | O6_2—H6C_2 | 0.848 (19) |
C4_1—H4B_1 | 0.9900 | O6_2—H6D_2 | 0.846 (18) |
C5_1—O3_1 | 1.429 (6) | O7_2—H7C_2 | 0.833 (18) |
C5_1—C6_1 | 1.499 (7) | O7_2—H7D_2 | 0.835 (18) |
C5_1—H5A_1 | 0.9900 | O8_2—H8C_2 | 0.812 (19) |
C5_1—H5B_1 | 0.9900 | O8_2—H8D_2 | 0.822 (19) |
C6_1—O4_1 | 1.435 (5) | O9_2—H9C_2 | 0.849 (19) |
C6_1—H6A_1 | 0.9900 | O9_2—H9D_2 | 0.836 (19) |
C6_1—H6B_1 | 0.9900 | O10_2—H10C_2 | 0.821 (19) |
C7_1—O4_1 | 1.425 (5) | O10_2—H10D_2 | 0.837 (19) |
C7_1—C8_1 | 1.504 (6) | O11_2—H11C_2 | 0.843 (19) |
C7_1—H7A_1 | 0.9900 | O11_2—H11D_2 | 0.835 (18) |
C7_1—H7B_1 | 0.9900 | N1_2—O12_2 | 1.249 (5) |
C8_1—O5_1 | 1.424 (6) | N1_2—O14_2 | 1.250 (5) |
C8_1—H8A_1 | 0.9900 | N1_2—O13_2 | 1.258 (5) |
C8_1—H8B_1 | 0.9900 | N2_2—O17_2 | 1.244 (5) |
C9_1—O5_1 | 1.429 (5) | N2_2—O16_2 | 1.255 (5) |
C9_1—C10_1 | 1.498 (7) | N2_2—O15_2 | 1.260 (5) |
C9_1—H9A_1 | 0.9900 | O18_2—H18C_2 | 0.838 (10) |
C9_1—H9B_1 | 0.9900 | O18_2—H18D_2 | 0.837 (10) |
C10_1—O1_1 | 1.422 (5) | C1_3—O1_3 | 1.428 (5) |
C10_1—H10A_1 | 0.9900 | C1_3—C2_3 | 1.497 (6) |
C10_1—H10B_1 | 0.9900 | C1_3—H1A_3 | 0.9900 |
Ni1_1—O11_1 | 2.032 (3) | C1_3—H1B_3 | 0.9900 |
Ni1_1—O6_1 | 2.033 (3) | C2_3—O2_3 | 1.438 (5) |
Ni1_1—O7_1 | 2.043 (3) | C2_3—H2A_3 | 0.9900 |
Ni1_1—O8_1 | 2.049 (4) | C2_3—H2B_3 | 0.9900 |
Ni1_1—O10_1 | 2.059 (4) | C3_3—O2_3 | 1.431 (5) |
Ni1_1—O9_1 | 2.060 (4) | C3_3—C4_3 | 1.481 (7) |
O6_1—H6C_1 | 0.840 (19) | C3_3—H3A_3 | 0.9900 |
O6_1—H6D_1 | 0.825 (18) | C3_3—H3B_3 | 0.9900 |
O7_1—H7C_1 | 0.829 (18) | C4_3—O3_3 | 1.434 (6) |
O7_1—H7D_1 | 0.834 (18) | C4_3—H4A_3 | 0.9900 |
O8_1—H8C_1 | 0.851 (19) | C4_3—H4B_3 | 0.9900 |
O8_1—H8D_1 | 0.834 (19) | C5_3—O3_3 | 1.426 (6) |
O9_1—H9C_1 | 0.824 (19) | C5_3—C6_3 | 1.507 (7) |
O9_1—H9D_1 | 0.851 (19) | C5_3—H5A_3 | 0.9900 |
O10_1—H10C_1 | 0.836 (19) | C5_3—H5B_3 | 0.9900 |
O10_1—H10D_1 | 0.839 (19) | C6_3—O4_3 | 1.425 (5) |
O11_1—H11C_1 | 0.839 (19) | C6_3—H6A_3 | 0.9900 |
O11_1—H11D_1 | 0.843 (19) | C6_3—H6B_3 | 0.9900 |
N1_1—O14_1 | 1.241 (5) | C7_3—O4_3 | 1.425 (5) |
N1_1—O13_1 | 1.254 (5) | C7_3—C8_3 | 1.501 (7) |
N1_1—O12_1 | 1.266 (5) | C7_3—H7A_3 | 0.9900 |
N2_1—O15_1 | 1.243 (5) | C7_3—H7B_3 | 0.9900 |
N2_1—O16_1 | 1.250 (5) | C8_3—O5_3 | 1.423 (5) |
N2_1—O17_1 | 1.258 (5) | C8_3—H8A_3 | 0.9900 |
N3_1—O20_1 | 1.240 (8) | C8_3—H8B_3 | 0.9900 |
N3_1—O19_1 | 1.249 (8) | C9_3—O5_3 | 1.448 (6) |
N3_1—O21_1 | 1.254 (8) | C9_3—C10_3 | 1.490 (6) |
N3'_1—O20'_1 | 1.242 (8) | C9_3—H9A_3 | 0.9900 |
N3'_1—O19'_1 | 1.250 (8) | C9_3—H9B_3 | 0.9900 |
N3'_1—O21'_1 | 1.257 (8) | C10_3—O1_3 | 1.438 (5) |
O18_1—H18C_1 | 0.845 (10) | C10_3—H10A_3 | 0.9900 |
O18_1—H18D_1 | 0.844 (10) | C10_3—H10B_3 | 0.9900 |
C1_2—O1_2 | 1.420 (6) | Ni3_3—O6_3i | 2.023 (3) |
C1_2—C2_2 | 1.495 (7) | Ni3_3—O6_3 | 2.023 (3) |
C1_2—H1A_2 | 0.9900 | Ni3_3—O9_3i | 2.039 (3) |
C1_2—H1B_2 | 0.9900 | Ni3_3—O9_3 | 2.039 (3) |
C2_2—O2_2 | 1.428 (5) | Ni3_3—O8_3 | 2.063 (3) |
C2_2—H2A_2 | 0.9900 | Ni3_3—O8_3i | 2.063 (3) |
C2_2—H2B_2 | 0.9900 | O6_3—H6C_3 | 0.835 (18) |
C3_2—O2_2 | 1.435 (6) | O6_3—H6D_3 | 0.812 (18) |
C3_2—C4_2 | 1.494 (7) | O8_3—H8C_3 | 0.835 (18) |
C3_2—H3A_2 | 0.9900 | O8_3—H8D_3 | 0.836 (18) |
C3_2—H3B_2 | 0.9900 | O9_3—H9C_3 | 0.845 (18) |
C4_2—O3_2 | 1.432 (6) | O9_3—H9D_3 | 0.831 (18) |
C4_2—H4A_2 | 0.9900 | Ni4_3—O10_3 | 2.018 (3) |
C4_2—H4B_2 | 0.9900 | Ni4_3—O10_3ii | 2.019 (3) |
C5_2—O3_2 | 1.423 (6) | Ni4_3—O7_3ii | 2.054 (3) |
C5_2—C6_2 | 1.508 (7) | Ni4_3—O7_3 | 2.054 (3) |
C5_2—H5A_2 | 0.9900 | Ni4_3—O11_3ii | 2.066 (3) |
C5_2—H5B_2 | 0.9900 | Ni4_3—O11_3 | 2.066 (3) |
C6_2—O4_2 | 1.431 (5) | O7_3—H7C_3 | 0.837 (18) |
C6_2—H6A_2 | 0.9900 | O7_3—H7D_3 | 0.837 (18) |
C6_2—H6B_2 | 0.9900 | O10_3—H10C_3 | 0.840 (19) |
C7_2—O4_2 | 1.424 (6) | O10_3—H10D_3 | 0.838 (19) |
C7_2—C8_2 | 1.496 (6) | O11_3—H11C_3 | 0.833 (18) |
C7_2—H7A_2 | 0.9900 | O11_3—H11D_3 | 0.834 (18) |
C7_2—H7B_2 | 0.9900 | N1_3—O13_3 | 1.244 (5) |
C8_2—O5_2 | 1.422 (6) | N1_3—O12_3 | 1.253 (5) |
C8_2—H8A_2 | 0.9900 | N1_3—O14_3 | 1.271 (5) |
C8_2—H8B_2 | 0.9900 | O18_3—H18C_3 | 0.833 (10) |
C9_2—O5_2 | 1.431 (5) | O18_3—H18D_3 | 0.828 (10) |
| | | |
O1_1—C1_1—C2_1 | 108.4 (4) | C9_2—C10_2—H10A_2 | 109.9 |
O1_1—C1_1—H1A_1 | 110.0 | O1_2—C10_2—H10B_2 | 109.9 |
C2_1—C1_1—H1A_1 | 110.0 | C9_2—C10_2—H10B_2 | 109.9 |
O1_1—C1_1—H1B_1 | 110.0 | H10A_2—C10_2—H10B_2 | 108.3 |
C2_1—C1_1—H1B_1 | 110.0 | C10_2—O1_2—C1_2 | 115.0 (4) |
H1A_1—C1_1—H1B_1 | 108.4 | C2_2—O2_2—C3_2 | 111.3 (4) |
O2_1—C2_1—C1_1 | 108.2 (4) | C5_2—O3_2—C4_2 | 114.4 (4) |
O2_1—C2_1—H2A_1 | 110.1 | C7_2—O4_2—C6_2 | 114.0 (4) |
C1_1—C2_1—H2A_1 | 110.1 | C8_2—O5_2—C9_2 | 114.4 (3) |
O2_1—C2_1—H2B_1 | 110.1 | O11_2—Ni2_2—O7_2 | 90.87 (13) |
C1_1—C2_1—H2B_1 | 110.1 | O11_2—Ni2_2—O9_2 | 174.99 (14) |
H2A_1—C2_1—H2B_1 | 108.4 | O7_2—Ni2_2—O9_2 | 86.88 (13) |
O2_1—C3_1—C4_1 | 113.2 (4) | O11_2—Ni2_2—O10_2 | 86.91 (13) |
O2_1—C3_1—H3A_1 | 108.9 | O7_2—Ni2_2—O10_2 | 90.25 (14) |
C4_1—C3_1—H3A_1 | 108.9 | O9_2—Ni2_2—O10_2 | 88.62 (14) |
O2_1—C3_1—H3B_1 | 108.9 | O11_2—Ni2_2—O6_2 | 91.18 (13) |
C4_1—C3_1—H3B_1 | 108.9 | O7_2—Ni2_2—O6_2 | 177.34 (14) |
H3A_1—C3_1—H3B_1 | 107.7 | O9_2—Ni2_2—O6_2 | 91.21 (13) |
O3_1—C4_1—C3_1 | 109.1 (4) | O10_2—Ni2_2—O6_2 | 91.55 (14) |
O3_1—C4_1—H4A_1 | 109.9 | O11_2—Ni2_2—O8_2 | 93.09 (14) |
C3_1—C4_1—H4A_1 | 109.9 | O7_2—Ni2_2—O8_2 | 89.51 (14) |
O3_1—C4_1—H4B_1 | 109.9 | O9_2—Ni2_2—O8_2 | 91.37 (14) |
C3_1—C4_1—H4B_1 | 109.9 | O10_2—Ni2_2—O8_2 | 179.76 (15) |
H4A_1—C4_1—H4B_1 | 108.3 | O6_2—Ni2_2—O8_2 | 88.68 (14) |
O3_1—C5_1—C6_1 | 109.1 (4) | Ni2_2—O6_2—H6C_2 | 130 (3) |
O3_1—C5_1—H5A_1 | 109.9 | Ni2_2—O6_2—H6D_2 | 124 (3) |
C6_1—C5_1—H5A_1 | 109.9 | H6C_2—O6_2—H6D_2 | 101 (3) |
O3_1—C5_1—H5B_1 | 109.9 | Ni2_2—O7_2—H7C_2 | 115 (3) |
C6_1—C5_1—H5B_1 | 109.9 | Ni2_2—O7_2—H7D_2 | 127 (3) |
H5A_1—C5_1—H5B_1 | 108.3 | H7C_2—O7_2—H7D_2 | 104 (3) |
O4_1—C6_1—C5_1 | 107.8 (4) | Ni2_2—O8_2—H8C_2 | 116 (3) |
O4_1—C6_1—H6A_1 | 110.2 | Ni2_2—O8_2—H8D_2 | 129 (3) |
C5_1—C6_1—H6A_1 | 110.2 | H8C_2—O8_2—H8D_2 | 110 (3) |
O4_1—C6_1—H6B_1 | 110.2 | Ni2_2—O9_2—H9C_2 | 120 (3) |
C5_1—C6_1—H6B_1 | 110.2 | Ni2_2—O9_2—H9D_2 | 114 (3) |
H6A_1—C6_1—H6B_1 | 108.5 | H9C_2—O9_2—H9D_2 | 103 (3) |
O4_1—C7_1—C8_1 | 107.7 (4) | Ni2_2—O10_2—H10C_2 | 123 (3) |
O4_1—C7_1—H7A_1 | 110.2 | Ni2_2—O10_2—H10D_2 | 129 (3) |
C8_1—C7_1—H7A_1 | 110.2 | H10C_2—O10_2—H10D_2 | 107 (3) |
O4_1—C7_1—H7B_1 | 110.2 | Ni2_2—O11_2—H11C_2 | 125 (3) |
C8_1—C7_1—H7B_1 | 110.2 | Ni2_2—O11_2—H11D_2 | 106 (3) |
H7A_1—C7_1—H7B_1 | 108.5 | H11C_2—O11_2—H11D_2 | 105 (3) |
O5_1—C8_1—C7_1 | 108.5 (4) | O12_2—N1_2—O14_2 | 121.7 (4) |
O5_1—C8_1—H8A_1 | 110.0 | O12_2—N1_2—O13_2 | 119.5 (4) |
C7_1—C8_1—H8A_1 | 110.0 | O14_2—N1_2—O13_2 | 118.8 (4) |
O5_1—C8_1—H8B_1 | 110.0 | O17_2—N2_2—O16_2 | 121.4 (4) |
C7_1—C8_1—H8B_1 | 110.0 | O17_2—N2_2—O15_2 | 119.7 (4) |
H8A_1—C8_1—H8B_1 | 108.4 | O16_2—N2_2—O15_2 | 119.0 (4) |
O5_1—C9_1—C10_1 | 108.5 (4) | H18C_2—O18_2—H18D_2 | 104.2 (16) |
O5_1—C9_1—H9A_1 | 110.0 | O1_3—C1_3—C2_3 | 108.8 (4) |
C10_1—C9_1—H9A_1 | 110.0 | O1_3—C1_3—H1A_3 | 109.9 |
O5_1—C9_1—H9B_1 | 110.0 | C2_3—C1_3—H1A_3 | 109.9 |
C10_1—C9_1—H9B_1 | 110.0 | O1_3—C1_3—H1B_3 | 109.9 |
H9A_1—C9_1—H9B_1 | 108.4 | C2_3—C1_3—H1B_3 | 109.9 |
O1_1—C10_1—C9_1 | 107.7 (4) | H1A_3—C1_3—H1B_3 | 108.3 |
O1_1—C10_1—H10A_1 | 110.2 | O2_3—C2_3—C1_3 | 108.0 (4) |
C9_1—C10_1—H10A_1 | 110.2 | O2_3—C2_3—H2A_3 | 110.1 |
O1_1—C10_1—H10B_1 | 110.2 | C1_3—C2_3—H2A_3 | 110.1 |
C9_1—C10_1—H10B_1 | 110.2 | O2_3—C2_3—H2B_3 | 110.1 |
H10A_1—C10_1—H10B_1 | 108.5 | C1_3—C2_3—H2B_3 | 110.1 |
C10_1—O1_1—C1_1 | 114.0 (4) | H2A_3—C2_3—H2B_3 | 108.4 |
C3_1—O2_1—C2_1 | 113.7 (4) | O2_3—C3_3—C4_3 | 108.8 (4) |
C5_1—O3_1—C4_1 | 112.4 (3) | O2_3—C3_3—H3A_3 | 109.9 |
C7_1—O4_1—C6_1 | 114.5 (3) | C4_3—C3_3—H3A_3 | 109.9 |
C8_1—O5_1—C9_1 | 114.1 (3) | O2_3—C3_3—H3B_3 | 109.9 |
O11_1—Ni1_1—O6_1 | 94.46 (13) | C4_3—C3_3—H3B_3 | 109.9 |
O11_1—Ni1_1—O7_1 | 88.51 (13) | H3A_3—C3_3—H3B_3 | 108.3 |
O6_1—Ni1_1—O7_1 | 174.74 (14) | O3_3—C4_3—C3_3 | 108.6 (4) |
O11_1—Ni1_1—O8_1 | 89.76 (16) | O3_3—C4_3—H4A_3 | 110.0 |
O6_1—Ni1_1—O8_1 | 90.13 (14) | C3_3—C4_3—H4A_3 | 110.0 |
O7_1—Ni1_1—O8_1 | 85.54 (14) | O3_3—C4_3—H4B_3 | 110.0 |
O11_1—Ni1_1—O10_1 | 87.76 (14) | C3_3—C4_3—H4B_3 | 110.0 |
O6_1—Ni1_1—O10_1 | 89.34 (14) | H4A_3—C4_3—H4B_3 | 108.4 |
O7_1—Ni1_1—O10_1 | 95.11 (14) | O3_3—C5_3—C6_3 | 107.7 (4) |
O8_1—Ni1_1—O10_1 | 177.42 (16) | O3_3—C5_3—H5A_3 | 110.2 |
O11_1—Ni1_1—O9_1 | 177.02 (17) | C6_3—C5_3—H5A_3 | 110.2 |
O6_1—Ni1_1—O9_1 | 87.01 (15) | O3_3—C5_3—H5B_3 | 110.2 |
O7_1—Ni1_1—O9_1 | 90.22 (15) | C6_3—C5_3—H5B_3 | 110.2 |
O8_1—Ni1_1—O9_1 | 92.8 (2) | H5A_3—C5_3—H5B_3 | 108.5 |
O10_1—Ni1_1—O9_1 | 89.67 (19) | O4_3—C6_3—C5_3 | 107.4 (4) |
Ni1_1—O6_1—H6C_1 | 120 (3) | O4_3—C6_3—H6A_3 | 110.2 |
Ni1_1—O6_1—H6D_1 | 128 (3) | C5_3—C6_3—H6A_3 | 110.2 |
H6C_1—O6_1—H6D_1 | 106 (3) | O4_3—C6_3—H6B_3 | 110.2 |
Ni1_1—O7_1—H7C_1 | 119 (3) | C5_3—C6_3—H6B_3 | 110.2 |
Ni1_1—O7_1—H7D_1 | 128 (3) | H6A_3—C6_3—H6B_3 | 108.5 |
H7C_1—O7_1—H7D_1 | 106 (3) | O4_3—C7_3—C8_3 | 107.9 (4) |
Ni1_1—O8_1—H8C_1 | 117 (4) | O4_3—C7_3—H7A_3 | 110.1 |
Ni1_1—O8_1—H8D_1 | 126 (4) | C8_3—C7_3—H7A_3 | 110.1 |
H8C_1—O8_1—H8D_1 | 104 (3) | O4_3—C7_3—H7B_3 | 110.1 |
Ni1_1—O9_1—H9C_1 | 123 (5) | C8_3—C7_3—H7B_3 | 110.1 |
Ni1_1—O9_1—H9D_1 | 105 (5) | H7A_3—C7_3—H7B_3 | 108.4 |
H9C_1—O9_1—H9D_1 | 104 (3) | O5_3—C8_3—C7_3 | 108.8 (4) |
Ni1_1—O10_1—H10C_1 | 113 (4) | O5_3—C8_3—H8A_3 | 109.9 |
Ni1_1—O10_1—H10D_1 | 117 (4) | C7_3—C8_3—H8A_3 | 109.9 |
H10C_1—O10_1—H10D_1 | 105 (3) | O5_3—C8_3—H8B_3 | 109.9 |
Ni1_1—O11_1—H11C_1 | 125 (3) | C7_3—C8_3—H8B_3 | 109.9 |
Ni1_1—O11_1—H11D_1 | 125 (3) | H8A_3—C8_3—H8B_3 | 108.3 |
H11C_1—O11_1—H11D_1 | 104 (3) | O5_3—C9_3—C10_3 | 107.7 (4) |
O14_1—N1_1—O13_1 | 120.2 (4) | O5_3—C9_3—H9A_3 | 110.2 |
O14_1—N1_1—O12_1 | 119.7 (5) | C10_3—C9_3—H9A_3 | 110.2 |
O13_1—N1_1—O12_1 | 120.0 (4) | O5_3—C9_3—H9B_3 | 110.2 |
O15_1—N2_1—O16_1 | 119.4 (4) | C10_3—C9_3—H9B_3 | 110.2 |
O15_1—N2_1—O17_1 | 120.9 (4) | H9A_3—C9_3—H9B_3 | 108.5 |
O16_1—N2_1—O17_1 | 119.7 (4) | O1_3—C10_3—C9_3 | 112.5 (4) |
O20_1—N3_1—O19_1 | 119.6 (9) | O1_3—C10_3—H10A_3 | 109.1 |
O20_1—N3_1—O21_1 | 120.7 (9) | C9_3—C10_3—H10A_3 | 109.1 |
O19_1—N3_1—O21_1 | 119.7 (9) | O1_3—C10_3—H10B_3 | 109.1 |
O20'_1—N3'_1—O19'_1 | 119.4 (10) | C9_3—C10_3—H10B_3 | 109.1 |
O20'_1—N3'_1—O21'_1 | 120.4 (10) | H10A_3—C10_3—H10B_3 | 107.8 |
O19'_1—N3'_1—O21'_1 | 120.3 (10) | C1_3—O1_3—C10_3 | 114.1 (3) |
H18C_1—O18_1—H18D_1 | 102.4 (16) | C3_3—O2_3—C2_3 | 112.9 (3) |
O1_2—C1_2—C2_2 | 108.1 (4) | C5_3—O3_3—C4_3 | 114.8 (3) |
O1_2—C1_2—H1A_2 | 110.1 | C7_3—O4_3—C6_3 | 113.2 (4) |
C2_2—C1_2—H1A_2 | 110.1 | C8_3—O5_3—C9_3 | 113.8 (3) |
O1_2—C1_2—H1B_2 | 110.1 | O6_3i—Ni3_3—O6_3 | 180.0 |
C2_2—C1_2—H1B_2 | 110.1 | O6_3i—Ni3_3—O9_3i | 90.79 (13) |
H1A_2—C1_2—H1B_2 | 108.4 | O6_3—Ni3_3—O9_3i | 89.21 (13) |
O2_2—C2_2—C1_2 | 108.5 (4) | O6_3i—Ni3_3—O9_3 | 89.21 (13) |
O2_2—C2_2—H2A_2 | 110.0 | O6_3—Ni3_3—O9_3 | 90.79 (13) |
C1_2—C2_2—H2A_2 | 110.0 | O9_3i—Ni3_3—O9_3 | 180.0 |
O2_2—C2_2—H2B_2 | 110.0 | O6_3i—Ni3_3—O8_3 | 88.78 (13) |
C1_2—C2_2—H2B_2 | 110.0 | O6_3—Ni3_3—O8_3 | 91.23 (13) |
H2A_2—C2_2—H2B_2 | 108.4 | O9_3i—Ni3_3—O8_3 | 86.11 (13) |
O2_2—C3_2—C4_2 | 108.0 (4) | O9_3—Ni3_3—O8_3 | 93.89 (13) |
O2_2—C3_2—H3A_2 | 110.1 | O6_3i—Ni3_3—O8_3i | 91.22 (13) |
C4_2—C3_2—H3A_2 | 110.1 | O6_3—Ni3_3—O8_3i | 88.77 (13) |
O2_2—C3_2—H3B_2 | 110.1 | O9_3i—Ni3_3—O8_3i | 93.89 (13) |
C4_2—C3_2—H3B_2 | 110.1 | O9_3—Ni3_3—O8_3i | 86.11 (13) |
H3A_2—C3_2—H3B_2 | 108.4 | O8_3—Ni3_3—O8_3i | 180.0 |
O3_2—C4_2—C3_2 | 112.1 (4) | Ni3_3—O6_3—H6C_3 | 116 (3) |
O3_2—C4_2—H4A_2 | 109.2 | Ni3_3—O6_3—H6D_3 | 130 (3) |
C3_2—C4_2—H4A_2 | 109.2 | H6C_3—O6_3—H6D_3 | 107 (3) |
O3_2—C4_2—H4B_2 | 109.2 | Ni3_3—O8_3—H8C_3 | 117 (3) |
C3_2—C4_2—H4B_2 | 109.2 | Ni3_3—O8_3—H8D_3 | 131 (3) |
H4A_2—C4_2—H4B_2 | 107.9 | H8C_3—O8_3—H8D_3 | 105 (3) |
O3_2—C5_2—C6_2 | 108.8 (4) | Ni3_3—O9_3—H9C_3 | 118 (3) |
O3_2—C5_2—H5A_2 | 109.9 | Ni3_3—O9_3—H9D_3 | 113 (3) |
C6_2—C5_2—H5A_2 | 109.9 | H9C_3—O9_3—H9D_3 | 104 (3) |
O3_2—C5_2—H5B_2 | 109.9 | O10_3—Ni4_3—O10_3ii | 180.0 |
C6_2—C5_2—H5B_2 | 109.9 | O10_3—Ni4_3—O7_3ii | 89.99 (15) |
H5A_2—C5_2—H5B_2 | 108.3 | O10_3ii—Ni4_3—O7_3ii | 90.02 (15) |
O4_2—C6_2—C5_2 | 107.8 (4) | O10_3—Ni4_3—O7_3 | 90.01 (15) |
O4_2—C6_2—H6A_2 | 110.1 | O10_3ii—Ni4_3—O7_3 | 89.99 (15) |
C5_2—C6_2—H6A_2 | 110.1 | O7_3ii—Ni4_3—O7_3 | 179.998 (1) |
O4_2—C6_2—H6B_2 | 110.1 | O10_3—Ni4_3—O11_3ii | 91.03 (14) |
C5_2—C6_2—H6B_2 | 110.1 | O10_3ii—Ni4_3—O11_3ii | 88.97 (14) |
H6A_2—C6_2—H6B_2 | 108.5 | O7_3ii—Ni4_3—O11_3ii | 90.36 (13) |
O4_2—C7_2—C8_2 | 107.5 (4) | O7_3—Ni4_3—O11_3ii | 89.64 (13) |
O4_2—C7_2—H7A_2 | 110.2 | O10_3—Ni4_3—O11_3 | 88.97 (14) |
C8_2—C7_2—H7A_2 | 110.2 | O10_3ii—Ni4_3—O11_3 | 91.03 (14) |
O4_2—C7_2—H7B_2 | 110.2 | O7_3ii—Ni4_3—O11_3 | 89.64 (13) |
C8_2—C7_2—H7B_2 | 110.2 | O7_3—Ni4_3—O11_3 | 90.36 (13) |
H7A_2—C7_2—H7B_2 | 108.5 | O11_3ii—Ni4_3—O11_3 | 179.999 (2) |
O5_2—C8_2—C7_2 | 108.5 (4) | Ni4_3—O7_3—H7C_3 | 118 (3) |
O5_2—C8_2—H8A_2 | 110.0 | Ni4_3—O7_3—H7D_3 | 118 (3) |
C7_2—C8_2—H8A_2 | 110.0 | H7C_3—O7_3—H7D_3 | 105 (3) |
O5_2—C8_2—H8B_2 | 110.0 | Ni4_3—O10_3—H10C_3 | 124 (3) |
C7_2—C8_2—H8B_2 | 110.0 | Ni4_3—O10_3—H10D_3 | 129 (3) |
H8A_2—C8_2—H8B_2 | 108.4 | H10C_3—O10_3—H10D_3 | 104 (3) |
O5_2—C9_2—C10_2 | 108.6 (4) | Ni4_3—O11_3—H11C_3 | 122 (3) |
O5_2—C9_2—H9A_2 | 110.0 | Ni4_3—O11_3—H11D_3 | 127 (3) |
C10_2—C9_2—H9A_2 | 110.0 | H11C_3—O11_3—H11D_3 | 105 (3) |
O5_2—C9_2—H9B_2 | 110.0 | O13_3—N1_3—O12_3 | 121.5 (4) |
C10_2—C9_2—H9B_2 | 110.0 | O13_3—N1_3—O14_3 | 119.7 (4) |
H9A_2—C9_2—H9B_2 | 108.4 | O12_3—N1_3—O14_3 | 118.8 (4) |
O1_2—C10_2—C9_2 | 109.0 (4) | H18C_3—O18_3—H18D_3 | 105.7 (17) |
O1_2—C10_2—H10A_2 | 109.9 | | |
| | | |
O1_1—C1_1—C2_1—O2_1 | −71.7 (5) | C4_2—C3_2—O2_2—C2_2 | 176.4 (4) |
O2_1—C3_1—C4_1—O3_1 | −58.0 (5) | C6_2—C5_2—O3_2—C4_2 | −170.3 (4) |
O3_1—C5_1—C6_1—O4_1 | 72.2 (5) | C3_2—C4_2—O3_2—C5_2 | 83.4 (5) |
O4_1—C7_1—C8_1—O5_1 | −66.2 (5) | C8_2—C7_2—O4_2—C6_2 | 178.0 (4) |
O5_1—C9_1—C10_1—O1_1 | 61.3 (5) | C5_2—C6_2—O4_2—C7_2 | −168.7 (4) |
C9_1—C10_1—O1_1—C1_1 | 174.4 (4) | C7_2—C8_2—O5_2—C9_2 | 163.9 (4) |
C2_1—C1_1—O1_1—C10_1 | 167.2 (4) | C10_2—C9_2—O5_2—C8_2 | −159.4 (4) |
C4_1—C3_1—O2_1—C2_1 | −80.4 (5) | O1_3—C1_3—C2_3—O2_3 | 76.3 (5) |
C1_1—C2_1—O2_1—C3_1 | 167.4 (4) | O2_3—C3_3—C4_3—O3_3 | −65.7 (5) |
C6_1—C5_1—O3_1—C4_1 | −163.7 (4) | O3_3—C5_3—C6_3—O4_3 | 62.3 (5) |
C3_1—C4_1—O3_1—C5_1 | −175.4 (4) | O4_3—C7_3—C8_3—O5_3 | −73.1 (4) |
C8_1—C7_1—O4_1—C6_1 | 165.1 (4) | O5_3—C9_3—C10_3—O1_3 | 60.7 (5) |
C5_1—C6_1—O4_1—C7_1 | −165.6 (4) | C2_3—C1_3—O1_3—C10_3 | −173.5 (4) |
C7_1—C8_1—O5_1—C9_1 | 160.9 (4) | C9_3—C10_3—O1_3—C1_3 | 95.8 (5) |
C10_1—C9_1—O5_1—C8_1 | −163.0 (4) | C4_3—C3_3—O2_3—C2_3 | 172.0 (4) |
O1_2—C1_2—C2_2—O2_2 | −67.5 (5) | C1_3—C2_3—O2_3—C3_3 | −166.1 (4) |
O2_2—C3_2—C4_2—O3_2 | 59.0 (6) | C6_3—C5_3—O3_3—C4_3 | −161.5 (4) |
O3_2—C5_2—C6_2—O4_2 | 75.1 (5) | C3_3—C4_3—O3_3—C5_3 | 160.1 (4) |
O4_2—C7_2—C8_2—O5_2 | −60.8 (5) | C8_3—C7_3—O4_3—C6_3 | −179.2 (4) |
O5_2—C9_2—C10_2—O1_2 | 64.6 (5) | C5_3—C6_3—O4_3—C7_3 | −176.4 (4) |
C9_2—C10_2—O1_2—C1_2 | −173.0 (4) | C7_3—C8_3—O5_3—C9_3 | 150.4 (4) |
C2_2—C1_2—O1_2—C10_2 | 166.7 (4) | C10_3—C9_3—O5_3—C8_3 | −172.5 (4) |
C1_2—C2_2—O2_2—C3_2 | 160.8 (4) | | |
Symmetry codes: (i) −x, −y, −z; (ii) −x+1, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O6_1—H6C_1···O3_1 | 0.84 (2) | 1.97 (2) | 2.792 (4) | 167 (5) |
O6_1—H6D_1···O5_1 | 0.83 (2) | 1.96 (2) | 2.767 (4) | 165 (5) |
O7_1—H7C_1···O1_2iii | 0.83 (2) | 1.97 (2) | 2.797 (5) | 172 (5) |
O7_1—H7D_1···O4_2iii | 0.83 (2) | 1.88 (2) | 2.711 (4) | 173 (5) |
O8_1—H8C_1···O2_1 | 0.85 (2) | 1.93 (2) | 2.766 (5) | 169 (6) |
O6_2—H6D_2···O2_2 | 0.85 (2) | 2.03 (2) | 2.870 (4) | 175 (4) |
O6_2—H6C_2···O5_2 | 0.85 (2) | 2.00 (2) | 2.815 (4) | 160 (5) |
O7_2—H7D_2···O1_1 | 0.84 (2) | 1.89 (2) | 2.717 (4) | 173 (5) |
O7_2—H7C_2···O4_1 | 0.83 (2) | 1.93 (2) | 2.752 (4) | 169 (5) |
O9_2—H9D_2···O3_2 | 0.84 (2) | 1.93 (2) | 2.754 (4) | 167 (5) |
O6_3—H6C_3···O1_3 | 0.84 (2) | 1.93 (2) | 2.753 (4) | 168 (5) |
O6_3—H6D_3···O3_3 | 0.81 (2) | 1.99 (2) | 2.788 (4) | 166 (5) |
O7_3—H7D_3···O2_3ii | 0.84 (2) | 1.94 (2) | 2.771 (4) | 171 (5) |
O7_3—H7C_3···O4_3ii | 0.84 (2) | 1.96 (2) | 2.780 (5) | 167 (5) |
O8_3—H8C_3···O5_3i | 0.84 (2) | 1.98 (2) | 2.810 (4) | 174 (5) |
O8_1—H8D_1···O19_1 | 0.83 (2) | 1.84 (3) | 2.650 (9) | 164 (5) |
O9_1—H9C_1···O20_1iv | 0.82 (2) | 2.32 (6) | 2.887 (14) | 126 (5) |
O9_1—H9C_1···O20′_1 | 0.82 (2) | 2.14 (4) | 2.771 (12) | 134 (6) |
O10_1—H10C_1···O12_1 | 0.84 (2) | 2.10 (3) | 2.867 (5) | 151 (4) |
O10_1—H10D_1···O17_1 | 0.84 (2) | 1.93 (2) | 2.745 (5) | 164 (5) |
O11_1—H11D_1···O15_1 | 0.84 (2) | 1.91 (2) | 2.746 (5) | 176 (5) |
O11_1—H11C_1···O18_1 | 0.84 (2) | 1.86 (2) | 2.690 (5) | 168 (5) |
O8_2—H8C_2···O12_1v | 0.81 (2) | 2.03 (2) | 2.834 (5) | 170 (5) |
O9_2—H9C_2···O13_1v | 0.85 (2) | 1.96 (2) | 2.797 (5) | 168 (5) |
O10_2—H10C_2···O14_2 | 0.82 (2) | 2.03 (2) | 2.838 (5) | 169 (4) |
O10_2—H10D_2···O18_2 | 0.84 (2) | 1.92 (2) | 2.727 (5) | 161 (5) |
O11_2—H11C_2···O12_2 | 0.84 (2) | 1.91 (2) | 2.746 (5) | 174 (4) |
O11_2—H11D_2···O15_2 | 0.84 (2) | 1.92 (3) | 2.693 (5) | 154 (5) |
O8_3—H8D_3···O13_2vi | 0.84 (2) | 1.94 (2) | 2.770 (4) | 174 (4) |
O9_3—H9C_3···O14_3i | 0.85 (2) | 1.94 (2) | 2.777 (4) | 171 (5) |
O9_3—H9D_3···O18_3i | 0.83 (2) | 1.96 (2) | 2.764 (5) | 161 (4) |
O10_3—H10C_3···O12_3v | 0.84 (2) | 1.87 (2) | 2.702 (5) | 168 (6) |
O10_3—H10D_3···O16_2ii | 0.84 (2) | 1.86 (2) | 2.669 (5) | 163 (5) |
O11_3—H11C_3···O13_3v | 0.83 (2) | 1.99 (2) | 2.822 (5) | 175 (5) |
O11_3—H11D_3···O16_1v | 0.83 (2) | 2.02 (2) | 2.848 (5) | 176 (5) |
Symmetry codes: (i) −x, −y, −z; (ii) −x+1, −y, −z; (iii) x−1, y, z; (iv) −x, −y+1, −z+1; (v) x, y, z−1; (vi) −x+1, −y, −z+1. |
Crystal data top
C10H20O5·C2H16NiO6·2(NO3)·C10H20O5·H12NiO6·2(NO3) | F(000) = 1112 |
Mr = 1050.22 | Dx = 1.548 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 5368 reflections |
a = 16.241 (1) Å | θ = 1.0–27.5° |
b = 15.481 (1) Å | µ = 0.94 mm−1 |
c = 10.429 (1) Å | T = 90 K |
β = 120.75 (1)° | Irregular block, pale green |
V = 2253.5 (4) Å3 | 0.20 × 0.15 × 0.11 mm |
Z = 2 | |
Data collection top
Nonius KappaCCD diffractometer | 5174 independent reflections |
Radiation source: fine-focus sealed tube | 3430 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
Detector resolution: 18 pixels mm-1 | θmax = 27.5°, θmin = 2.0° |
ω scans at fixed χ = 55° | h = −21→21 |
Absorption correction: multi-scan Scalepack (Otwinowski & Minor, 2006) | k = −20→20 |
Tmin = 0.834, Tmax = 0.903 | l = −13→13 |
10144 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.037 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.101 | H 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 parameters | Δρmax = 0.71 e Å−3 |
51 restraints | Δρmin = −0.51 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C1 | 0.2556 (5) | −0.1809 (4) | −0.0093 (5) | 0.0224 (11) | 0.575 (3) |
H1A | 0.2080 | −0.2076 | 0.0110 | 0.027* | 0.575 (3) |
H1B | 0.3047 | −0.2247 | 0.0082 | 0.027* | 0.575 (3) |
C2 | 0.2074 (7) | −0.1493 (5) | −0.1673 (6) | 0.0222 (12) | 0.575 (3) |
H2A | 0.2541 | −0.1187 | −0.1853 | 0.027* | 0.575 (3) |
H2B | 0.1808 | −0.1986 | −0.2373 | 0.027* | 0.575 (3) |
C3 | 0.0934 (4) | −0.0406 (5) | −0.3240 (9) | 0.0290 (14) | 0.575 (3) |
H3A | 0.0273 | −0.0241 | −0.3523 | 0.035* | 0.575 (3) |
H3B | 0.0886 | −0.0779 | −0.4046 | 0.035* | 0.575 (3) |
C10 | 0.3189 (4) | −0.1213 (4) | 0.2342 (5) | 0.0301 (12) | 0.575 (3) |
H10A | 0.3567 | −0.1747 | 0.2769 | 0.036* | 0.575 (3) |
H10B | 0.2584 | −0.1264 | 0.2351 | 0.036* | 0.575 (3) |
O1 | 0.29969 (19) | −0.10765 (17) | 0.0869 (3) | 0.0243 (8) | 0.575 (3) |
O2 | 0.13244 (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) |
H1'1 | 0.2932 | −0.2343 | 0.0643 | 0.027* | 0.425 (3) |
H1'2 | 0.3415 | −0.1425 | 0.0710 | 0.027* | 0.425 (3) |
C2' | 0.2121 (10) | −0.1605 (6) | −0.1250 (9) | 0.0222 (12) | 0.425 (3) |
H2'1 | 0.2353 | −0.1933 | −0.1819 | 0.027* | 0.425 (3) |
H2'2 | 0.1478 | −0.1825 | −0.1530 | 0.027* | 0.425 (3) |
C3' | 0.1222 (7) | −0.0493 (6) | −0.3006 (12) | 0.0290 (14) | 0.425 (3) |
H3'1 | 0.0634 | −0.0519 | −0.2945 | 0.035* | 0.425 (3) |
H3'2 | 0.1152 | −0.0878 | −0.3813 | 0.035* | 0.425 (3) |
C10' | 0.3005 (5) | −0.1207 (5) | 0.2723 (7) | 0.0301 (12) | 0.425 (3) |
H10C | 0.3371 | −0.1746 | 0.3156 | 0.036* | 0.425 (3) |
H10D | 0.2617 | −0.1107 | 0.3195 | 0.036* | 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) |
C4 | 0.14547 (18) | 0.03982 (17) | −0.3203 (3) | 0.0309 (6) | |
H4A | 0.2113 | 0.0253 | −0.2957 | 0.037* | |
H4B | 0.1120 | 0.0681 | −0.4194 | 0.037* | |
C5 | 0.19807 (16) | 0.17591 (15) | −0.1985 (2) | 0.0229 (5) | |
H5A | 0.1561 | 0.2150 | −0.2819 | 0.028* | |
H5B | 0.2563 | 0.1639 | −0.2033 | 0.028* | |
C6 | 0.22495 (15) | 0.21744 (15) | −0.0523 (2) | 0.0207 (5) | |
H6A | 0.2495 | 0.2766 | −0.0477 | 0.025* | |
H6B | 0.1683 | 0.2212 | −0.0405 | 0.025* | |
C7 | 0.31257 (15) | 0.18047 (14) | 0.2085 (2) | 0.0183 (5) | |
H7A | 0.2505 | 0.1824 | 0.2050 | 0.022* | |
H7B | 0.3456 | 0.2364 | 0.2476 | 0.022* | |
C8 | 0.37293 (15) | 0.10806 (14) | 0.3069 (2) | 0.0211 (5) | |
H8A | 0.4313 | 0.1015 | 0.3002 | 0.025* | |
H8B | 0.3928 | 0.1204 | 0.4120 | 0.025* | |
C9 | 0.37305 (16) | −0.04593 (15) | 0.3188 (3) | 0.0264 (6) | |
H9A | 0.3910 | −0.0524 | 0.4244 | 0.032* | |
H9B | 0.4326 | −0.0413 | 0.3153 | 0.032* | |
O3 | 0.14881 (10) | 0.09710 (10) | −0.21010 (16) | 0.0210 (4) | |
O4 | 0.29728 (10) | 0.16516 (9) | 0.06293 (15) | 0.0178 (3) | |
O5 | 0.31728 (10) | 0.03030 (10) | 0.25838 (16) | 0.0211 (4) | |
Ni1 | 0.5000 | 0.0000 | 0.0000 | 0.01354 (11) | |
O7 | 0.62612 (11) | −0.02569 (11) | 0.00679 (19) | 0.0242 (4) | |
H7C | 0.6421 (17) | −0.0696 (11) | −0.022 (3) | 0.036* | |
H7D | 0.6614 (16) | 0.0121 (12) | 0.017 (3) | 0.036* | |
O8 | 0.42130 (12) | −0.07295 (11) | −0.18908 (17) | 0.0248 (4) | |
H8C | 0.3871 (15) | −0.0493 (14) | −0.271 (2) | 0.037* | |
H8D | 0.4431 (17) | −0.1166 (12) | −0.203 (3) | 0.037* | |
O9 | 0.51406 (11) | −0.10859 (10) | 0.12079 (17) | 0.0200 (3) | |
H9C | 0.5175 (16) | −0.1557 (12) | 0.084 (2) | 0.030* | |
H9D | 0.5602 (14) | −0.1092 (14) | 0.2100 (17) | 0.030* | |
Ni2 | 0.0000 | 0.0000 | 0.0000 | 0.01295 (11) | |
O6 | 0.12290 (10) | 0.05293 (10) | 0.02445 (17) | 0.0183 (3) | |
H6C | 0.1270 (15) | 0.0663 (14) | −0.0502 (18) | 0.027* | |
H6D | 0.1757 (12) | 0.0367 (15) | 0.0895 (19) | 0.027* | |
O10 | 0.06786 (12) | −0.02105 (11) | 0.22246 (17) | 0.0253 (4) | |
H10E | 0.1105 (16) | 0.0132 (12) | 0.282 (2) | 0.038* | |
H10F | 0.0745 (17) | −0.0677 (11) | 0.263 (3) | 0.038* | |
O11 | 0.04652 (11) | −0.11770 (10) | −0.03048 (18) | 0.0219 (4) | |
H11D | 0.0753 (16) | −0.1081 (16) | −0.069 (3) | 0.033* | |
C11 | −0.00716 (16) | −0.19561 (14) | −0.0769 (3) | 0.0262 (6) | |
H11A | −0.0176 | −0.2165 | 0.0024 | 0.039* | |
H11B | 0.0282 | −0.2392 | −0.0977 | 0.039* | |
H11C | −0.0691 | −0.1849 | −0.1674 | 0.039* | |
N1 | 0.46460 (13) | 0.27268 (12) | 0.1179 (2) | 0.0210 (4) | |
O12 | 0.46900 (12) | 0.25755 (10) | 0.00340 (17) | 0.0316 (4) | |
O13 | 0.41547 (10) | 0.33478 (9) | 0.11782 (16) | 0.0247 (4) | |
O14 | 0.50915 (10) | 0.22561 (10) | 0.23208 (16) | 0.0208 (3) | |
N2 | 0.72821 (13) | −0.07374 (13) | 0.48854 (19) | 0.0209 (4) | |
O15 | 0.66587 (11) | −0.12709 (10) | 0.40313 (17) | 0.0290 (4) | |
O16 | 0.80361 (11) | −0.10068 (10) | 0.60019 (16) | 0.0241 (4) | |
O17 | 0.71584 (13) | 0.00565 (9) | 0.46263 (18) | 0.0232 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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 | 0.0288 (17) | 0.0189 (16) | 0.0279 (15) | −0.0051 (13) | 0.0164 (13) | −0.0053 (12) |
O2 | 0.0196 (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) |
C4 | 0.0322 (14) | 0.0419 (16) | 0.0226 (13) | −0.0045 (13) | 0.0170 (11) | −0.0076 (12) |
C5 | 0.0194 (12) | 0.0276 (14) | 0.0227 (12) | −0.0006 (10) | 0.0115 (10) | 0.0065 (10) |
C6 | 0.0176 (11) | 0.0173 (12) | 0.0251 (12) | 0.0036 (10) | 0.0093 (9) | 0.0061 (10) |
C7 | 0.0211 (12) | 0.0196 (12) | 0.0184 (11) | −0.0011 (9) | 0.0131 (10) | −0.0024 (9) |
C8 | 0.0181 (11) | 0.0246 (13) | 0.0208 (12) | −0.0039 (10) | 0.0101 (10) | −0.0002 (10) |
C9 | 0.0260 (13) | 0.0274 (15) | 0.0270 (13) | 0.0092 (11) | 0.0144 (11) | 0.0102 (11) |
O3 | 0.0203 (8) | 0.0260 (9) | 0.0185 (8) | −0.0033 (7) | 0.0113 (7) | −0.0032 (7) |
O4 | 0.0170 (8) | 0.0189 (8) | 0.0173 (8) | 0.0036 (6) | 0.0086 (7) | 0.0020 (6) |
O5 | 0.0198 (8) | 0.0168 (8) | 0.0246 (9) | 0.0030 (7) | 0.0100 (7) | 0.0033 (7) |
Ni1 | 0.0131 (2) | 0.0132 (2) | 0.0144 (2) | 0.00119 (15) | 0.00712 (16) | −0.00089 (15) |
O7 | 0.0198 (9) | 0.0214 (9) | 0.0372 (10) | −0.0015 (7) | 0.0186 (8) | −0.0081 (8) |
O8 | 0.0276 (9) | 0.0199 (9) | 0.0184 (8) | 0.0059 (7) | 0.0057 (7) | −0.0032 (7) |
O9 | 0.0227 (8) | 0.0158 (8) | 0.0176 (8) | 0.0015 (7) | 0.0076 (7) | 0.0001 (7) |
Ni2 | 0.0114 (2) | 0.0126 (2) | 0.0150 (2) | −0.00084 (15) | 0.00678 (16) | 0.00100 (15) |
O6 | 0.0152 (8) | 0.0226 (9) | 0.0174 (8) | −0.0021 (7) | 0.0085 (7) | 0.0022 (7) |
O10 | 0.0261 (9) | 0.0239 (10) | 0.0174 (9) | −0.0066 (7) | 0.0049 (7) | 0.0051 (7) |
O11 | 0.0199 (8) | 0.0184 (9) | 0.0326 (9) | −0.0004 (7) | 0.0170 (7) | −0.0012 (7) |
C11 | 0.0232 (13) | 0.0173 (13) | 0.0377 (14) | −0.0020 (10) | 0.0152 (11) | −0.0013 (11) |
N1 | 0.0210 (10) | 0.0145 (10) | 0.0251 (11) | −0.0020 (8) | 0.0100 (9) | −0.0029 (8) |
O12 | 0.0524 (11) | 0.0240 (10) | 0.0243 (9) | 0.0077 (8) | 0.0239 (8) | −0.0003 (7) |
O13 | 0.0244 (9) | 0.0154 (8) | 0.0326 (9) | 0.0025 (7) | 0.0133 (8) | −0.0048 (7) |
O14 | 0.0187 (8) | 0.0205 (8) | 0.0210 (8) | 0.0002 (7) | 0.0084 (7) | 0.0008 (7) |
N2 | 0.0242 (11) | 0.0222 (12) | 0.0173 (10) | 0.0014 (9) | 0.0112 (9) | 0.0007 (8) |
O15 | 0.0264 (9) | 0.0279 (10) | 0.0206 (8) | −0.0055 (8) | 0.0033 (7) | −0.0027 (7) |
O16 | 0.0196 (8) | 0.0264 (9) | 0.0177 (8) | 0.0026 (7) | 0.0033 (7) | 0.0026 (7) |
O17 | 0.0288 (9) | 0.0191 (10) | 0.0193 (8) | 0.0044 (7) | 0.0106 (7) | 0.0027 (7) |
Geometric parameters (Å, º) top
C1—O1 | 1.439 (6) | C7—H7A | 0.9900 |
C1—C2 | 1.500 (6) | C7—H7B | 0.9900 |
C1—H1A | 0.9900 | C8—O5 | 1.433 (3) |
C1—H1B | 0.9900 | C8—H8A | 0.9900 |
C2—O2 | 1.423 (8) | C8—H8B | 0.9900 |
C2—H2A | 0.9900 | C9—O5 | 1.424 (3) |
C2—H2B | 0.9900 | C9—H9A | 0.9900 |
C3—O2 | 1.443 (6) | C9—H9B | 0.9900 |
C3—C4 | 1.495 (7) | Ni1—O9 | 2.0423 (15) |
C3—H3A | 0.9900 | Ni1—O9i | 2.0423 (15) |
C3—H3B | 0.9900 | Ni1—O7 | 2.0519 (15) |
C10—O1 | 1.419 (5) | Ni1—O7i | 2.0521 (15) |
C10—C9 | 1.456 (5) | Ni1—O8 | 2.0543 (15) |
C10—H10A | 0.9900 | Ni1—O8i | 2.0543 (15) |
C10—H10B | 0.9900 | O7—H7C | 0.837 (15) |
C1'—O1' | 1.434 (10) | O7—H7D | 0.786 (15) |
C1'—C2' | 1.506 (8) | O8—H8C | 0.832 (15) |
C1'—H1'1 | 0.9900 | O8—H8D | 0.809 (15) |
C1'—H1'2 | 0.9900 | O9—H9C | 0.838 (15) |
C2'—O2' | 1.446 (10) | O9—H9D | 0.845 (15) |
C2'—H2'1 | 0.9900 | Ni2—O10 | 2.0221 (15) |
C2'—H2'2 | 0.9900 | Ni2—O10ii | 2.0221 (15) |
C3'—O2' | 1.444 (7) | Ni2—O6ii | 2.0494 (14) |
C3'—C4 | 1.472 (8) | Ni2—O6 | 2.0494 (14) |
C3'—H3'1 | 0.9900 | Ni2—O11 | 2.0586 (15) |
C3'—H3'2 | 0.9900 | Ni2—O11ii | 2.0587 (15) |
C10'—O1' | 1.441 (6) | O6—H6C | 0.840 (15) |
C10'—C9 | 1.543 (7) | O6—H6D | 0.815 (15) |
C10'—H10C | 0.9900 | O10—H10E | 0.839 (15) |
C10'—H10D | 0.9900 | O10—H10F | 0.817 (15) |
C4—O3 | 1.430 (3) | O11—C11 | 1.420 (3) |
C4—H4A | 0.9900 | O11—H11D | 0.773 (16) |
C4—H4B | 0.9900 | C11—H11A | 0.9800 |
C5—O3 | 1.430 (3) | C11—H11B | 0.9800 |
C5—C6 | 1.499 (3) | C11—H11C | 0.9800 |
C5—H5A | 0.9900 | N1—O13 | 1.249 (2) |
C5—H5B | 0.9900 | N1—O12 | 1.254 (2) |
C6—O4 | 1.427 (2) | N1—O14 | 1.262 (2) |
C6—H6A | 0.9900 | N2—O17 | 1.252 (2) |
C6—H6B | 0.9900 | N2—O16 | 1.253 (2) |
C7—O4 | 1.427 (2) | N2—O15 | 1.256 (2) |
C7—C8 | 1.497 (3) | | |
| | | |
O1—C1—C2 | 107.6 (6) | O5—C8—C7 | 108.25 (17) |
O1—C1—H1A | 110.2 | O5—C8—H8A | 110.0 |
C2—C1—H1A | 110.2 | C7—C8—H8A | 110.0 |
O1—C1—H1B | 110.2 | O5—C8—H8B | 110.0 |
C2—C1—H1B | 110.2 | C7—C8—H8B | 110.0 |
H1A—C1—H1B | 108.5 | H8A—C8—H8B | 108.4 |
O2—C2—C1 | 108.0 (5) | O5—C9—C10 | 110.2 (3) |
O2—C2—H2A | 110.1 | O5—C9—C10' | 105.8 (4) |
C1—C2—H2A | 110.1 | O5—C9—H9A | 109.6 |
O2—C2—H2B | 110.1 | C10—C9—H9A | 109.6 |
C1—C2—H2B | 110.1 | C10'—C9—H9A | 91.0 |
H2A—C2—H2B | 108.4 | O5—C9—H9B | 109.6 |
O2—C3—C4 | 118.2 (5) | C10—C9—H9B | 109.6 |
O2—C3—H3A | 107.8 | C10'—C9—H9B | 130.4 |
C4—C3—H3A | 107.8 | H9A—C9—H9B | 108.1 |
O2—C3—H3B | 107.8 | C5—O3—C4 | 112.75 (16) |
C4—C3—H3B | 107.8 | C6—O4—C7 | 114.97 (16) |
H3A—C3—H3B | 107.1 | C9—O5—C8 | 113.35 (16) |
O1—C10—C9 | 105.5 (4) | O9—Ni1—O9i | 179.997 (1) |
O1—C10—H10A | 110.6 | O9—Ni1—O7 | 91.40 (7) |
C9—C10—H10A | 110.6 | O9i—Ni1—O7 | 88.60 (7) |
O1—C10—H10B | 110.6 | O9—Ni1—O7i | 88.60 (7) |
C9—C10—H10B | 110.7 | O9i—Ni1—O7i | 91.39 (7) |
H10A—C10—H10B | 108.8 | O7—Ni1—O7i | 180.0 |
C10—O1—C1 | 113.1 (4) | O9—Ni1—O8 | 87.60 (6) |
C2—O2—C3 | 114.9 (5) | O9i—Ni1—O8 | 92.40 (6) |
O1'—C1'—C2' | 107.4 (8) | O7—Ni1—O8 | 92.68 (7) |
O1'—C1'—H1'1 | 110.2 | O7i—Ni1—O8 | 87.32 (7) |
C2'—C1'—H1'1 | 110.2 | O9—Ni1—O8i | 92.40 (6) |
O1'—C1'—H1'2 | 110.2 | O9i—Ni1—O8i | 87.59 (6) |
C2'—C1'—H1'2 | 110.2 | O7—Ni1—O8i | 87.32 (7) |
H1'1—C1'—H1'2 | 108.5 | O7i—Ni1—O8i | 92.67 (7) |
O2'—C2'—C1' | 108.4 (8) | O8—Ni1—O8i | 180.0 |
O2'—C2'—H2'1 | 110.0 | Ni1—O7—H7C | 129.3 (17) |
C1'—C2'—H2'1 | 110.0 | Ni1—O7—H7D | 120.2 (18) |
O2'—C2'—H2'2 | 110.0 | H7C—O7—H7D | 108 (2) |
C1'—C2'—H2'2 | 110.0 | Ni1—O8—H8C | 120.5 (17) |
H2'1—C2'—H2'2 | 108.4 | Ni1—O8—H8D | 121.0 (18) |
O2'—C3'—C4 | 99.6 (5) | H8C—O8—H8D | 108 (2) |
O2'—C3'—H3'1 | 111.8 | Ni1—O9—H9C | 116.7 (16) |
C4—C3'—H3'1 | 111.8 | Ni1—O9—H9D | 116.4 (16) |
O2'—C3'—H3'2 | 111.8 | H9C—O9—H9D | 105.2 (18) |
C4—C3'—H3'2 | 111.8 | O10—Ni2—O10ii | 180.0 |
H3'1—C3'—H3'2 | 109.6 | O10—Ni2—O6ii | 90.18 (6) |
O1'—C10'—C9 | 118.4 (5) | O10ii—Ni2—O6ii | 89.82 (6) |
O1'—C10'—H10C | 107.7 | O10—Ni2—O6 | 89.82 (6) |
C9—C10'—H10C | 107.7 | O10ii—Ni2—O6 | 90.18 (6) |
O1'—C10'—H10D | 107.7 | O6ii—Ni2—O6 | 180.0 |
C9—C10'—H10D | 107.7 | O10—Ni2—O11 | 90.39 (7) |
H10C—C10'—H10D | 107.1 | O10ii—Ni2—O11 | 89.61 (7) |
C1'—O1'—C10' | 113.8 (5) | O6ii—Ni2—O11 | 92.17 (6) |
C3'—O2'—C2' | 111.6 (6) | O6—Ni2—O11 | 87.83 (6) |
O3—C4—C3' | 112.1 (6) | O10—Ni2—O11ii | 89.61 (7) |
O3—C4—C3 | 109.0 (4) | O10ii—Ni2—O11ii | 90.39 (7) |
O3—C4—H4A | 109.9 | O6ii—Ni2—O11ii | 87.83 (6) |
C3'—C4—H4A | 94.1 | O6—Ni2—O11ii | 92.17 (6) |
C3—C4—H4A | 109.9 | O11—Ni2—O11ii | 180.0 |
O3—C4—H4B | 109.9 | Ni2—O6—H6C | 121.1 (15) |
C3'—C4—H4B | 121.1 | Ni2—O6—H6D | 121.6 (16) |
C3—C4—H4B | 109.9 | H6C—O6—H6D | 107.4 (19) |
H4A—C4—H4B | 108.3 | Ni2—O10—H10E | 120.1 (17) |
O3—C5—C6 | 108.15 (17) | Ni2—O10—H10F | 126.1 (17) |
O3—C5—H5A | 110.1 | H10E—O10—H10F | 110 (2) |
C6—C5—H5A | 110.1 | C11—O11—Ni2 | 126.47 (12) |
O3—C5—H5B | 110.1 | C11—O11—H11D | 114.5 (19) |
C6—C5—H5B | 110.1 | Ni2—O11—H11D | 106.2 (19) |
H5A—C5—H5B | 108.4 | O11—C11—H11A | 109.5 |
O4—C6—C5 | 107.42 (18) | O11—C11—H11B | 109.5 |
O4—C6—H6A | 110.2 | H11A—C11—H11B | 109.5 |
C5—C6—H6A | 110.2 | O11—C11—H11C | 109.5 |
O4—C6—H6B | 110.2 | H11A—C11—H11C | 109.5 |
C5—C6—H6B | 110.2 | H11B—C11—H11C | 109.5 |
H6A—C6—H6B | 108.5 | O13—N1—O12 | 119.38 (18) |
O4—C7—C8 | 107.55 (17) | O13—N1—O14 | 120.18 (17) |
O4—C7—H7A | 110.2 | O12—N1—O14 | 120.43 (18) |
C8—C7—H7A | 110.2 | O17—N2—O16 | 119.98 (19) |
O4—C7—H7B | 110.2 | O17—N2—O15 | 120.66 (18) |
C8—C7—H7B | 110.2 | O16—N2—O15 | 119.36 (19) |
H7A—C7—H7B | 108.5 | | |
| | | |
O1—C1—C2—O2 | −64.6 (8) | O1—C10—C9—O5 | 61.4 (4) |
C9—C10—O1—C1 | 173.3 (4) | O1—C10—C9—C10' | 144.3 (15) |
C2—C1—O1—C10 | 159.6 (6) | O1'—C10'—C9—O5 | 59.4 (6) |
C1—C2—O2—C3 | 166.3 (6) | O1'—C10'—C9—C10 | −45.3 (9) |
C4—C3—O2—C2 | −82.2 (9) | C6—C5—O3—C4 | −162.14 (19) |
O1'—C1'—C2'—O2' | 68.9 (11) | C3'—C4—O3—C5 | 162.4 (4) |
C2'—C1'—O1'—C10' | −164.2 (7) | C3—C4—O3—C5 | 179.7 (3) |
C9—C10'—O1'—C1' | 72.4 (8) | C5—C6—O4—C7 | −163.26 (17) |
C4—C3'—O2'—C2' | −169.0 (7) | C8—C7—O4—C6 | 167.32 (17) |
C1'—C2'—O2'—C3' | −160.9 (10) | C10—C9—O5—C8 | −163.6 (3) |
O2'—C3'—C4—O3 | −65.9 (9) | C10'—C9—O5—C8 | 172.5 (3) |
O2'—C3'—C4—C3 | −148 (4) | C7—C8—O5—C9 | 165.81 (17) |
O2—C3—C4—O3 | −60.8 (7) | O10—Ni2—O11—C11 | 99.27 (17) |
O2—C3—C4—C3' | 43 (3) | O10ii—Ni2—O11—C11 | −80.73 (17) |
O3—C5—C6—O4 | 69.2 (2) | O6ii—Ni2—O11—C11 | 9.08 (17) |
O4—C7—C8—O5 | −67.6 (2) | O6—Ni2—O11—C11 | −170.92 (17) |
Symmetry codes: (i) −x+1, −y, −z; (ii) −x, −y, −z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7C···O4i | 0.84 (2) | 1.94 (2) | 2.768 (2) | 170 (2) |
O7—H7D···O2′i | 0.79 (2) | 2.08 (2) | 2.765 (4) | 146 (3) |
O7—H7D···O1i | 0.79 (2) | 2.11 (2) | 2.806 (3) | 147 (3) |
O8—H8C···O17i | 0.83 (2) | 1.96 (2) | 2.773 (2) | 168 (2) |
O8—H8D···O14i | 0.81 (2) | 1.95 (2) | 2.753 (2) | 176 (3) |
O9—H9C···O12i | 0.84 (2) | 1.89 (2) | 2.727 (2) | 175 (2) |
O9—H9D···O15 | 0.85 (2) | 1.88 (2) | 2.722 (2) | 172 (2) |
O6—H6C···O3 | 0.84 (2) | 1.93 (2) | 2.771 (2) | 175 (2) |
O6—H6D···O5 | 0.82 (2) | 2.06 (2) | 2.857 (2) | 165 (2) |
O10—H10E···O16iii | 0.84 (2) | 1.88 (2) | 2.717 (2) | 173 (2) |
O10—H10F···O13iv | 0.82 (2) | 1.91 (2) | 2.714 (2) | 169 (3) |
O11—H11D···O2 | 0.77 (2) | 1.92 (2) | 2.692 (3) | 172 (3) |
O11—H11D···O1′ | 0.77 (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, y−1/2, −z+1/2. |
Crystal data top
C10H20O5·H8N2NiO10·C10H20O5·H8N2NiO10 | F(000) = 4000 |
Mr = 950.11 | Dx = 1.644 Mg m−3 |
Orthorhombic, Pbca | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2ab | Cell parameters from 9379 reflections |
a = 15.352 (1) Å | θ = 1.0–27.5° |
b = 16.278 (1) Å | µ = 1.09 mm−1 |
c = 30.716 (2) Å | T = 90 K |
V = 7675.9 (8) Å3 | Plate, pale green |
Z = 8 | 0.50 × 0.40 × 0.05 mm |
Data collection top
Nonius KappaCCD diffractometer | 8782 independent reflections |
Radiation source: fine-focus sealed tube | 6081 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.044 |
Detector resolution: 18 pixels mm-1 | θmax = 27.5°, θmin = 1.3° |
ω scans at fixed χ = 55° | h = −19→19 |
Absorption correction: multi-scan Scalepack (Otwinowski & Minor, 2006) | k = −21→21 |
Tmin = 0.612, Tmax = 0.948 | l = −39→39 |
16396 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.079 | H 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 parameters | Δρmax = 0.33 e Å−3 |
24 restraints | Δρmin = −0.49 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
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 | x | y | z | Uiso*/Ueq | |
C1_1 | 0.14539 (15) | 0.16617 (14) | 0.06705 (7) | 0.0195 (6) | |
H1A_1 | 0.0817 | 0.1754 | 0.0665 | 0.023* | |
H1B_1 | 0.1622 | 0.1493 | 0.0969 | 0.023* | |
C2_1 | 0.16971 (15) | 0.10065 (15) | 0.03516 (8) | 0.0203 (6) | |
H2A_1 | 0.1339 | 0.0509 | 0.0401 | 0.024* | |
H2B_1 | 0.1594 | 0.1201 | 0.0051 | 0.024* | |
C3_1 | 0.29823 (14) | 0.04043 (14) | 0.00473 (7) | 0.0151 (5) | |
H3A_1 | 0.2798 | 0.0671 | −0.0227 | 0.018* | |
H3B_1 | 0.2790 | −0.0176 | 0.0041 | 0.018* | |
C4_1 | 0.39568 (15) | 0.04472 (13) | 0.00931 (7) | 0.0145 (5) | |
H4A_1 | 0.4140 | 0.0196 | 0.0372 | 0.017* | |
H4B_1 | 0.4241 | 0.0145 | −0.0148 | 0.017* | |
C5_1 | 0.50952 (14) | 0.14529 (13) | 0.01824 (7) | 0.0144 (5) | |
H5A_1 | 0.5474 | 0.1262 | −0.0058 | 0.017* | |
H5B_1 | 0.5265 | 0.1159 | 0.0452 | 0.017* | |
C6_1 | 0.51933 (15) | 0.23604 (14) | 0.02440 (7) | 0.0147 (5) | |
H6A_1 | 0.5814 | 0.2500 | 0.0292 | 0.018* | |
H6B_1 | 0.4989 | 0.2654 | −0.0019 | 0.018* | |
C7_1 | 0.45482 (16) | 0.34689 (13) | 0.06255 (8) | 0.0187 (5) | |
H7A_1 | 0.4221 | 0.3645 | 0.0364 | 0.022* | |
H7B_1 | 0.5114 | 0.3760 | 0.0629 | 0.022* | |
C8_1 | 0.40388 (15) | 0.36749 (14) | 0.10302 (8) | 0.0187 (5) | |
H8A_1 | 0.4391 | 0.3532 | 0.1290 | 0.022* | |
H8B_1 | 0.3926 | 0.4274 | 0.1038 | 0.022* | |
C9_1 | 0.25254 (15) | 0.36402 (14) | 0.08258 (7) | 0.0190 (5) | |
H9A_1 | 0.2690 | 0.3752 | 0.0520 | 0.023* | |
H9B_1 | 0.2383 | 0.4169 | 0.0969 | 0.023* | |
C10_1 | 0.17564 (15) | 0.30740 (15) | 0.08417 (7) | 0.0199 (6) | |
H10A_1 | 0.1674 | 0.2868 | 0.1142 | 0.024* | |
H10B_1 | 0.1223 | 0.3374 | 0.0755 | 0.024* | |
O1_1 | 0.19023 (10) | 0.23990 (10) | 0.05517 (5) | 0.0193 (4) | |
O2_1 | 0.26007 (9) | 0.08184 (9) | 0.04116 (5) | 0.0160 (4) | |
O4_1 | 0.46875 (10) | 0.26024 (9) | 0.06134 (5) | 0.0141 (3) | |
O3_1 | 0.42025 (9) | 0.12940 (9) | 0.00819 (5) | 0.0134 (3) | |
O5_1 | 0.32250 (10) | 0.32442 (9) | 0.10487 (5) | 0.0160 (4) | |
Ni1_1 | 0.387899 (18) | 0.120446 (17) | 0.168692 (8) | 0.01125 (8) | |
O6_1 | 0.39832 (10) | 0.11150 (10) | 0.23501 (5) | 0.0134 (3) | |
H6C_1 | 0.3598 (12) | 0.0916 (13) | 0.2494 (7) | 0.020* | |
H6D_1 | 0.4228 (13) | 0.1474 (12) | 0.2486 (7) | 0.020* | |
O7_1 | 0.38128 (10) | 0.13049 (10) | 0.10288 (5) | 0.0143 (4) | |
H7C_1 | 0.3369 (12) | 0.1189 (14) | 0.0897 (7) | 0.021* | |
H7D_1 | 0.4020 (14) | 0.1724 (11) | 0.0918 (7) | 0.021* | |
O9_1 | 0.46923 (11) | 0.02073 (9) | 0.16578 (5) | 0.0157 (4) | |
H9C_1 | 0.4894 (14) | 0.0105 (14) | 0.1421 (6) | 0.024* | |
H9D_1 | 0.4347 (13) | −0.0179 (12) | 0.1713 (7) | 0.024* | |
O11_1 | 0.30554 (10) | 0.21920 (9) | 0.17369 (5) | 0.0137 (3) | |
H11C_1 | 0.3071 (15) | 0.2517 (13) | 0.1529 (5) | 0.021* | |
H11D_1 | 0.3203 (15) | 0.2485 (13) | 0.1951 (5) | 0.021* | |
N1_1 | 0.55316 (12) | 0.21331 (12) | 0.14650 (6) | 0.0148 (4) | |
O10_1 | 0.48648 (9) | 0.20875 (9) | 0.17088 (5) | 0.0139 (3) | |
O12_1 | 0.57758 (10) | 0.15271 (9) | 0.12493 (5) | 0.0157 (4) | |
O13_1 | 0.59262 (10) | 0.28071 (9) | 0.14543 (5) | 0.0181 (4) | |
N2_1 | 0.26347 (13) | −0.02339 (11) | 0.18283 (6) | 0.0167 (4) | |
O8_1 | 0.27490 (10) | 0.05012 (9) | 0.16881 (5) | 0.0164 (4) | |
O14_1 | 0.32834 (11) | −0.06858 (10) | 0.18961 (6) | 0.0265 (4) | |
O15_1 | 0.18864 (10) | −0.04778 (10) | 0.18921 (5) | 0.0232 (4) | |
C1_2 | 0.16985 (15) | 0.13064 (14) | 0.26939 (7) | 0.0168 (5) | |
H1A_2 | 0.1866 | 0.1203 | 0.2388 | 0.020* | |
H1B_2 | 0.1069 | 0.1436 | 0.2703 | 0.020* | |
C2_2 | 0.18859 (14) | 0.05635 (14) | 0.29668 (7) | 0.0168 (5) | |
H2A_2 | 0.1765 | 0.0685 | 0.3277 | 0.020* | |
H2B_2 | 0.1507 | 0.0102 | 0.2875 | 0.020* | |
C3_2 | 0.31373 (15) | −0.01046 (14) | 0.32739 (7) | 0.0164 (5) | |
H3A_2 | 0.2948 | −0.0685 | 0.3260 | 0.020* | |
H3B_2 | 0.2925 | 0.0134 | 0.3551 | 0.020* | |
C4_2 | 0.41098 (15) | −0.00585 (13) | 0.32567 (7) | 0.0178 (5) | |
H4A_2 | 0.4368 | −0.0415 | 0.3484 | 0.021* | |
H4B_2 | 0.4322 | −0.0246 | 0.2969 | 0.021* | |
C5_2 | 0.52594 (14) | 0.09339 (14) | 0.32642 (7) | 0.0162 (5) | |
H5A_2 | 0.5452 | 0.0705 | 0.2981 | 0.019* | |
H5B_2 | 0.5605 | 0.0673 | 0.3499 | 0.019* | |
C6_2 | 0.53881 (15) | 0.18459 (14) | 0.32709 (7) | 0.0150 (5) | |
H6A_2 | 0.5140 | 0.2079 | 0.3542 | 0.018* | |
H6B_2 | 0.6018 | 0.1976 | 0.3263 | 0.018* | |
C7_2 | 0.48296 (15) | 0.30636 (14) | 0.29414 (7) | 0.0171 (5) | |
H7A_2 | 0.5395 | 0.3350 | 0.2971 | 0.021* | |
H7B_2 | 0.4474 | 0.3183 | 0.3203 | 0.021* | |
C8_2 | 0.43624 (14) | 0.33491 (13) | 0.25355 (7) | 0.0166 (5) | |
H8A_2 | 0.4258 | 0.3948 | 0.2555 | 0.020* | |
H8B_2 | 0.4737 | 0.3247 | 0.2279 | 0.020* | |
C9_2 | 0.28370 (14) | 0.32793 (14) | 0.27203 (7) | 0.0160 (5) | |
H9A_2 | 0.2716 | 0.3845 | 0.2619 | 0.019* | |
H9B_2 | 0.2986 | 0.3301 | 0.3034 | 0.019* | |
C10_2 | 0.20495 (14) | 0.27471 (13) | 0.26520 (7) | 0.0162 (5) | |
H10A_2 | 0.1526 | 0.3019 | 0.2773 | 0.019* | |
H10B_2 | 0.1954 | 0.2655 | 0.2337 | 0.019* | |
O1_2 | 0.21936 (10) | 0.19793 (9) | 0.28671 (5) | 0.0170 (4) | |
O2_2 | 0.27822 (10) | 0.03428 (9) | 0.29129 (5) | 0.0148 (3) | |
O3_2 | 0.43523 (9) | 0.07774 (9) | 0.33284 (5) | 0.0143 (3) | |
O4_2 | 0.49642 (10) | 0.21979 (9) | 0.28999 (5) | 0.0147 (4) | |
O5_2 | 0.35481 (10) | 0.29357 (9) | 0.24779 (5) | 0.0152 (3) | |
Ni2_2 | 0.310559 (18) | 0.224144 (17) | 0.424075 (9) | 0.01100 (8) | |
O6_2 | 0.31286 (10) | 0.24637 (10) | 0.48896 (5) | 0.0142 (3) | |
H6C_2 | 0.2689 (11) | 0.2481 (14) | 0.5040 (7) | 0.021* | |
H6D_2 | 0.3441 (13) | 0.2865 (12) | 0.4962 (7) | 0.021* | |
O7_2 | 0.31825 (11) | 0.19572 (10) | 0.35948 (5) | 0.0165 (4) | |
H7C_2 | 0.2802 (12) | 0.1986 (14) | 0.3402 (7) | 0.025* | |
H7D_2 | 0.3539 (13) | 0.1613 (13) | 0.3528 (7) | 0.025* | |
O8_2 | 0.21410 (10) | 0.13883 (10) | 0.43534 (5) | 0.0157 (4) | |
H8C_2 | 0.2414 (14) | 0.0947 (11) | 0.4327 (7) | 0.024* | |
H8D_2 | 0.1763 (13) | 0.1397 (14) | 0.4160 (7) | 0.024* | |
O11_2 | 0.21665 (11) | 0.31105 (10) | 0.41521 (5) | 0.0162 (4) | |
H11C_2 | 0.1788 (13) | 0.3011 (13) | 0.3963 (7) | 0.024* | |
H11D_2 | 0.2432 (14) | 0.3516 (12) | 0.4071 (7) | 0.024* | |
N1_2 | 0.41446 (13) | 0.38312 (12) | 0.40661 (6) | 0.0149 (4) | |
O10_2 | 0.41505 (10) | 0.30683 (9) | 0.41585 (5) | 0.0140 (3) | |
O12_2 | 0.48439 (10) | 0.42195 (9) | 0.40797 (5) | 0.0181 (4) | |
O13_2 | 0.34503 (11) | 0.41863 (10) | 0.39621 (6) | 0.0262 (4) | |
N2_2 | 0.41339 (13) | 0.06660 (12) | 0.43212 (6) | 0.0166 (4) | |
O9_2 | 0.41386 (9) | 0.14503 (9) | 0.43280 (5) | 0.0140 (3) | |
O14_2 | 0.48365 (10) | 0.02978 (10) | 0.43117 (6) | 0.0246 (4) | |
O15_2 | 0.34260 (10) | 0.02762 (9) | 0.43221 (5) | 0.0193 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1_1 | 0.0139 (13) | 0.0239 (14) | 0.0206 (13) | −0.0033 (11) | 0.0032 (10) | 0.0028 (11) |
C2_1 | 0.0130 (13) | 0.0264 (15) | 0.0214 (13) | −0.0017 (11) | 0.0012 (10) | 0.0009 (11) |
C3_1 | 0.0188 (13) | 0.0140 (12) | 0.0126 (11) | −0.0025 (10) | −0.0022 (10) | −0.0008 (9) |
C4_1 | 0.0205 (13) | 0.0104 (12) | 0.0126 (11) | 0.0006 (10) | −0.0007 (10) | −0.0004 (9) |
C5_1 | 0.0131 (13) | 0.0174 (13) | 0.0127 (12) | 0.0024 (10) | 0.0007 (10) | −0.0004 (9) |
C6_1 | 0.0129 (12) | 0.0178 (13) | 0.0134 (12) | −0.0020 (10) | 0.0021 (10) | 0.0009 (10) |
C7_1 | 0.0214 (14) | 0.0117 (13) | 0.0230 (13) | −0.0025 (10) | 0.0021 (11) | 0.0005 (10) |
C8_1 | 0.0216 (14) | 0.0125 (13) | 0.0220 (13) | −0.0025 (10) | 0.0004 (11) | −0.0030 (10) |
C9_1 | 0.0257 (14) | 0.0181 (13) | 0.0132 (12) | 0.0074 (11) | −0.0026 (11) | 0.0005 (10) |
C10_1 | 0.0193 (14) | 0.0242 (14) | 0.0162 (12) | 0.0086 (11) | 0.0012 (10) | −0.0026 (10) |
O1_1 | 0.0201 (9) | 0.0222 (9) | 0.0156 (8) | −0.0033 (7) | 0.0056 (7) | −0.0024 (7) |
O2_1 | 0.0108 (8) | 0.0246 (9) | 0.0125 (8) | 0.0001 (7) | 0.0006 (7) | −0.0030 (7) |
O4_1 | 0.0185 (9) | 0.0109 (8) | 0.0129 (8) | 0.0010 (7) | 0.0031 (7) | −0.0013 (6) |
O3_1 | 0.0102 (8) | 0.0136 (8) | 0.0163 (8) | −0.0002 (7) | −0.0012 (7) | 0.0021 (6) |
O5_1 | 0.0170 (9) | 0.0138 (9) | 0.0172 (8) | −0.0001 (7) | −0.0023 (7) | 0.0022 (7) |
Ni1_1 | 0.01291 (16) | 0.01245 (15) | 0.00839 (14) | 0.00064 (12) | 0.00054 (12) | 0.00014 (12) |
O6_1 | 0.0168 (9) | 0.0153 (9) | 0.0081 (8) | −0.0040 (7) | 0.0011 (7) | 0.0000 (6) |
O7_1 | 0.0178 (9) | 0.0168 (9) | 0.0084 (8) | −0.0053 (7) | −0.0013 (7) | 0.0014 (7) |
O9_1 | 0.0182 (9) | 0.0152 (9) | 0.0138 (9) | 0.0021 (7) | 0.0050 (7) | −0.0002 (7) |
O11_1 | 0.0170 (9) | 0.0139 (9) | 0.0103 (8) | 0.0019 (7) | −0.0005 (7) | 0.0003 (6) |
N1_1 | 0.0119 (10) | 0.0220 (12) | 0.0103 (10) | 0.0002 (9) | −0.0027 (8) | 0.0019 (8) |
O10_1 | 0.0107 (8) | 0.0178 (9) | 0.0133 (8) | −0.0034 (7) | 0.0062 (7) | −0.0007 (7) |
O12_1 | 0.0161 (9) | 0.0177 (9) | 0.0134 (8) | 0.0036 (7) | 0.0030 (7) | −0.0018 (7) |
O13_1 | 0.0177 (9) | 0.0172 (9) | 0.0194 (9) | −0.0076 (7) | 0.0012 (7) | −0.0004 (7) |
N2_1 | 0.0217 (12) | 0.0159 (11) | 0.0126 (10) | −0.0006 (9) | 0.0015 (9) | 0.0012 (8) |
O8_1 | 0.0176 (9) | 0.0121 (8) | 0.0196 (9) | −0.0027 (7) | −0.0020 (7) | 0.0041 (7) |
O14_1 | 0.0206 (10) | 0.0170 (9) | 0.0420 (11) | 0.0051 (8) | 0.0040 (8) | 0.0093 (8) |
O15_1 | 0.0161 (9) | 0.0251 (10) | 0.0284 (10) | −0.0069 (8) | −0.0001 (8) | 0.0062 (8) |
C1_2 | 0.0116 (12) | 0.0211 (14) | 0.0178 (12) | −0.0016 (10) | −0.0013 (10) | −0.0056 (10) |
C2_2 | 0.0118 (12) | 0.0176 (13) | 0.0210 (13) | −0.0023 (10) | 0.0030 (10) | −0.0059 (10) |
C3_2 | 0.0229 (14) | 0.0128 (12) | 0.0137 (12) | −0.0040 (10) | −0.0017 (11) | 0.0009 (9) |
C4_2 | 0.0243 (14) | 0.0122 (12) | 0.0169 (12) | 0.0007 (10) | −0.0036 (11) | −0.0013 (10) |
C5_2 | 0.0133 (12) | 0.0218 (13) | 0.0135 (12) | −0.0013 (10) | 0.0004 (10) | 0.0019 (10) |
C6_2 | 0.0113 (12) | 0.0221 (13) | 0.0116 (11) | −0.0013 (10) | −0.0016 (10) | 0.0024 (10) |
C7_2 | 0.0173 (13) | 0.0137 (13) | 0.0204 (13) | −0.0009 (10) | 0.0017 (10) | −0.0052 (10) |
C8_2 | 0.0196 (13) | 0.0128 (12) | 0.0173 (12) | −0.0014 (10) | 0.0033 (10) | −0.0017 (10) |
C9_2 | 0.0191 (13) | 0.0162 (13) | 0.0128 (12) | 0.0048 (10) | 0.0011 (10) | 0.0008 (10) |
C10_2 | 0.0182 (13) | 0.0171 (13) | 0.0133 (12) | 0.0071 (10) | 0.0003 (10) | 0.0014 (10) |
O1_2 | 0.0225 (9) | 0.0140 (9) | 0.0144 (8) | −0.0016 (7) | −0.0073 (7) | 0.0012 (7) |
O2_2 | 0.0137 (8) | 0.0179 (9) | 0.0128 (8) | 0.0022 (7) | 0.0004 (7) | 0.0015 (7) |
O3_2 | 0.0132 (8) | 0.0131 (8) | 0.0167 (8) | −0.0028 (7) | 0.0003 (7) | −0.0021 (7) |
O4_2 | 0.0176 (9) | 0.0150 (9) | 0.0115 (8) | 0.0000 (7) | −0.0035 (7) | −0.0007 (6) |
O5_2 | 0.0154 (9) | 0.0158 (8) | 0.0143 (8) | 0.0024 (7) | 0.0000 (7) | −0.0027 (7) |
Ni2_2 | 0.01126 (15) | 0.01253 (16) | 0.00920 (14) | −0.00050 (12) | −0.00029 (12) | −0.00065 (11) |
O6_2 | 0.0128 (9) | 0.0185 (9) | 0.0112 (8) | −0.0048 (7) | 0.0015 (7) | −0.0031 (7) |
O7_2 | 0.0169 (10) | 0.0220 (10) | 0.0106 (8) | 0.0055 (7) | −0.0033 (7) | −0.0050 (7) |
O8_2 | 0.0129 (9) | 0.0163 (9) | 0.0178 (9) | −0.0001 (7) | −0.0026 (7) | −0.0011 (7) |
O11_2 | 0.0157 (9) | 0.0149 (9) | 0.0180 (9) | −0.0005 (7) | −0.0048 (7) | 0.0003 (7) |
N1_2 | 0.0186 (11) | 0.0166 (11) | 0.0096 (10) | −0.0023 (9) | −0.0010 (8) | 0.0003 (8) |
O10_2 | 0.0155 (9) | 0.0105 (8) | 0.0160 (8) | −0.0026 (7) | 0.0009 (7) | −0.0001 (6) |
O12_2 | 0.0146 (9) | 0.0182 (9) | 0.0216 (9) | −0.0080 (7) | 0.0000 (7) | 0.0030 (7) |
O13_2 | 0.0164 (9) | 0.0213 (10) | 0.0409 (11) | 0.0005 (8) | −0.0068 (8) | 0.0117 (8) |
N2_2 | 0.0196 (12) | 0.0139 (11) | 0.0163 (11) | 0.0020 (9) | −0.0024 (9) | 0.0014 (8) |
O9_2 | 0.0134 (8) | 0.0109 (8) | 0.0177 (8) | 0.0032 (7) | −0.0011 (7) | −0.0010 (6) |
O14_2 | 0.0155 (9) | 0.0154 (9) | 0.0427 (11) | 0.0066 (8) | −0.0024 (8) | 0.0030 (8) |
O15_2 | 0.0155 (9) | 0.0148 (9) | 0.0278 (10) | −0.0041 (7) | 0.0013 (7) | 0.0038 (7) |
Geometric parameters (Å, º) top
C1_1—O1_1 | 1.431 (3) | C1_2—O1_2 | 1.435 (3) |
C1_1—C2_1 | 1.496 (3) | C1_2—C2_2 | 1.499 (3) |
C1_1—H1A_1 | 0.9900 | C1_2—H1A_2 | 0.9900 |
C1_1—H1B_1 | 0.9900 | C1_2—H1B_2 | 0.9900 |
C2_1—O2_1 | 1.432 (3) | C2_2—O2_2 | 1.432 (3) |
C2_1—H2A_1 | 0.9900 | C2_2—H2A_2 | 0.9900 |
C2_1—H2B_1 | 0.9900 | C2_2—H2B_2 | 0.9900 |
C3_1—O2_1 | 1.432 (2) | C3_2—O2_2 | 1.434 (2) |
C3_1—C4_1 | 1.504 (3) | C3_2—C4_2 | 1.496 (3) |
C3_1—H3A_1 | 0.9900 | C3_2—H3A_2 | 0.9900 |
C3_1—H3B_1 | 0.9900 | C3_2—H3B_2 | 0.9900 |
C4_1—O3_1 | 1.429 (2) | C4_2—O3_2 | 1.428 (2) |
C4_1—H4A_1 | 0.9900 | C4_2—H4A_2 | 0.9900 |
C4_1—H4B_1 | 0.9900 | C4_2—H4B_2 | 0.9900 |
C5_1—O3_1 | 1.428 (3) | C5_2—O3_2 | 1.429 (3) |
C5_1—C6_1 | 1.497 (3) | C5_2—C6_2 | 1.498 (3) |
C5_1—H5A_1 | 0.9900 | C5_2—H5A_2 | 0.9900 |
C5_1—H5B_1 | 0.9900 | C5_2—H5B_2 | 0.9900 |
C6_1—O4_1 | 1.430 (2) | C6_2—O4_2 | 1.432 (2) |
C6_1—H6A_1 | 0.9900 | C6_2—H6A_2 | 0.9900 |
C6_1—H6B_1 | 0.9900 | C6_2—H6B_2 | 0.9900 |
C7_1—O4_1 | 1.427 (3) | C7_2—O4_2 | 1.430 (3) |
C7_1—C8_1 | 1.506 (3) | C7_2—C8_2 | 1.512 (3) |
C7_1—H7A_1 | 0.9900 | C7_2—H7A_2 | 0.9900 |
C7_1—H7B_1 | 0.9900 | C7_2—H7B_2 | 0.9900 |
C8_1—O5_1 | 1.434 (3) | C8_2—O5_2 | 1.431 (3) |
C8_1—H8A_1 | 0.9900 | C8_2—H8A_2 | 0.9900 |
C8_1—H8B_1 | 0.9900 | C8_2—H8B_2 | 0.9900 |
C9_1—O5_1 | 1.428 (3) | C9_2—O5_2 | 1.435 (2) |
C9_1—C10_1 | 1.498 (3) | C9_2—C10_2 | 1.502 (3) |
C9_1—H9A_1 | 0.9900 | C9_2—H9A_2 | 0.9900 |
C9_1—H9B_1 | 0.9900 | C9_2—H9B_2 | 0.9900 |
C10_1—O1_1 | 1.432 (3) | C10_2—O1_2 | 1.431 (3) |
C10_1—H10A_1 | 0.9900 | C10_2—H10A_2 | 0.9900 |
C10_1—H10B_1 | 0.9900 | C10_2—H10B_2 | 0.9900 |
Ni1_1—O7_1 | 2.0307 (15) | Ni2_2—O6_2 | 2.0257 (15) |
Ni1_1—O6_1 | 2.0486 (14) | Ni2_2—O11_2 | 2.0381 (16) |
Ni1_1—O9_1 | 2.0498 (16) | Ni2_2—O7_2 | 2.0408 (15) |
Ni1_1—O11_1 | 2.0509 (15) | Ni2_2—O8_2 | 2.0594 (16) |
Ni1_1—O8_1 | 2.0784 (15) | Ni2_2—O9_2 | 2.0604 (15) |
Ni1_1—O10_1 | 2.0883 (15) | Ni2_2—O10_2 | 2.1092 (15) |
O6_1—H6C_1 | 0.806 (15) | O6_2—H6C_2 | 0.817 (15) |
O6_1—H6D_1 | 0.810 (15) | O6_2—H6D_2 | 0.840 (15) |
O7_1—H7C_1 | 0.814 (15) | O7_2—H7C_2 | 0.834 (15) |
O7_1—H7D_1 | 0.826 (15) | O7_2—H7D_2 | 0.810 (15) |
O9_1—H9C_1 | 0.809 (15) | O8_2—H8C_2 | 0.836 (15) |
O9_1—H9D_1 | 0.840 (15) | O8_2—H8D_2 | 0.831 (15) |
O11_1—H11C_1 | 0.830 (15) | O11_2—H11C_2 | 0.838 (15) |
O11_1—H11D_1 | 0.844 (15) | O11_2—H11D_2 | 0.815 (15) |
N1_1—O12_1 | 1.246 (2) | N1_2—O12_2 | 1.247 (2) |
N1_1—O13_1 | 1.254 (2) | N1_2—O13_2 | 1.254 (2) |
N1_1—O10_1 | 1.270 (2) | N1_2—O10_2 | 1.274 (2) |
N2_1—O15_1 | 1.231 (2) | N2_2—O14_2 | 1.234 (2) |
N2_1—O14_1 | 1.255 (2) | N2_2—O15_2 | 1.258 (2) |
N2_1—O8_1 | 1.284 (2) | N2_2—O9_2 | 1.277 (2) |
| | | |
O1_1—C1_1—C2_1 | 108.12 (18) | O1_2—C1_2—C2_2 | 107.86 (18) |
O1_1—C1_1—H1A_1 | 110.1 | O1_2—C1_2—H1A_2 | 110.1 |
C2_1—C1_1—H1A_1 | 110.1 | C2_2—C1_2—H1A_2 | 110.1 |
O1_1—C1_1—H1B_1 | 110.1 | O1_2—C1_2—H1B_2 | 110.1 |
C2_1—C1_1—H1B_1 | 110.1 | C2_2—C1_2—H1B_2 | 110.1 |
H1A_1—C1_1—H1B_1 | 108.4 | H1A_2—C1_2—H1B_2 | 108.4 |
O2_1—C2_1—C1_1 | 108.06 (18) | O2_2—C2_2—C1_2 | 108.79 (18) |
O2_1—C2_1—H2A_1 | 110.1 | O2_2—C2_2—H2A_2 | 109.9 |
C1_1—C2_1—H2A_1 | 110.1 | C1_2—C2_2—H2A_2 | 109.9 |
O2_1—C2_1—H2B_1 | 110.1 | O2_2—C2_2—H2B_2 | 109.9 |
C1_1—C2_1—H2B_1 | 110.1 | C1_2—C2_2—H2B_2 | 109.9 |
H2A_1—C2_1—H2B_1 | 108.4 | H2A_2—C2_2—H2B_2 | 108.3 |
O2_1—C3_1—C4_1 | 108.18 (17) | O2_2—C3_2—C4_2 | 109.06 (18) |
O2_1—C3_1—H3A_1 | 110.1 | O2_2—C3_2—H3A_2 | 109.9 |
C4_1—C3_1—H3A_1 | 110.1 | C4_2—C3_2—H3A_2 | 109.9 |
O2_1—C3_1—H3B_1 | 110.1 | O2_2—C3_2—H3B_2 | 109.9 |
C4_1—C3_1—H3B_1 | 110.1 | C4_2—C3_2—H3B_2 | 109.9 |
H3A_1—C3_1—H3B_1 | 108.4 | H3A_2—C3_2—H3B_2 | 108.3 |
O3_1—C4_1—C3_1 | 107.76 (18) | O3_2—C4_2—C3_2 | 107.62 (18) |
O3_1—C4_1—H4A_1 | 110.2 | O3_2—C4_2—H4A_2 | 110.2 |
C3_1—C4_1—H4A_1 | 110.2 | C3_2—C4_2—H4A_2 | 110.2 |
O3_1—C4_1—H4B_1 | 110.2 | O3_2—C4_2—H4B_2 | 110.2 |
C3_1—C4_1—H4B_1 | 110.2 | C3_2—C4_2—H4B_2 | 110.2 |
H4A_1—C4_1—H4B_1 | 108.5 | H4A_2—C4_2—H4B_2 | 108.5 |
O3_1—C5_1—C6_1 | 107.62 (18) | O3_2—C5_2—C6_2 | 107.65 (18) |
O3_1—C5_1—H5A_1 | 110.2 | O3_2—C5_2—H5A_2 | 110.2 |
C6_1—C5_1—H5A_1 | 110.2 | C6_2—C5_2—H5A_2 | 110.2 |
O3_1—C5_1—H5B_1 | 110.2 | O3_2—C5_2—H5B_2 | 110.2 |
C6_1—C5_1—H5B_1 | 110.2 | C6_2—C5_2—H5B_2 | 110.2 |
H5A_1—C5_1—H5B_1 | 108.5 | H5A_2—C5_2—H5B_2 | 108.5 |
O4_1—C6_1—C5_1 | 108.51 (17) | O4_2—C6_2—C5_2 | 109.01 (17) |
O4_1—C6_1—H6A_1 | 110.0 | O4_2—C6_2—H6A_2 | 109.9 |
C5_1—C6_1—H6A_1 | 110.0 | C5_2—C6_2—H6A_2 | 109.9 |
O4_1—C6_1—H6B_1 | 110.0 | O4_2—C6_2—H6B_2 | 109.9 |
C5_1—C6_1—H6B_1 | 110.0 | C5_2—C6_2—H6B_2 | 109.9 |
H6A_1—C6_1—H6B_1 | 108.4 | H6A_2—C6_2—H6B_2 | 108.3 |
O4_1—C7_1—C8_1 | 108.62 (18) | O4_2—C7_2—C8_2 | 107.33 (17) |
O4_1—C7_1—H7A_1 | 110.0 | O4_2—C7_2—H7A_2 | 110.2 |
C8_1—C7_1—H7A_1 | 110.0 | C8_2—C7_2—H7A_2 | 110.2 |
O4_1—C7_1—H7B_1 | 110.0 | O4_2—C7_2—H7B_2 | 110.2 |
C8_1—C7_1—H7B_1 | 110.0 | C8_2—C7_2—H7B_2 | 110.2 |
H7A_1—C7_1—H7B_1 | 108.3 | H7A_2—C7_2—H7B_2 | 108.5 |
O5_1—C8_1—C7_1 | 112.11 (18) | O5_2—C8_2—C7_2 | 111.84 (18) |
O5_1—C8_1—H8A_1 | 109.2 | O5_2—C8_2—H8A_2 | 109.2 |
C7_1—C8_1—H8A_1 | 109.2 | C7_2—C8_2—H8A_2 | 109.2 |
O5_1—C8_1—H8B_1 | 109.2 | O5_2—C8_2—H8B_2 | 109.2 |
C7_1—C8_1—H8B_1 | 109.2 | C7_2—C8_2—H8B_2 | 109.2 |
H8A_1—C8_1—H8B_1 | 107.9 | H8A_2—C8_2—H8B_2 | 107.9 |
O5_1—C9_1—C10_1 | 107.42 (18) | O5_2—C9_2—C10_2 | 108.36 (17) |
O5_1—C9_1—H9A_1 | 110.2 | O5_2—C9_2—H9A_2 | 110.0 |
C10_1—C9_1—H9A_1 | 110.2 | C10_2—C9_2—H9A_2 | 110.0 |
O5_1—C9_1—H9B_1 | 110.2 | O5_2—C9_2—H9B_2 | 110.0 |
C10_1—C9_1—H9B_1 | 110.2 | C10_2—C9_2—H9B_2 | 110.0 |
H9A_1—C9_1—H9B_1 | 108.5 | H9A_2—C9_2—H9B_2 | 108.4 |
O1_1—C10_1—C9_1 | 109.17 (18) | O1_2—C10_2—C9_2 | 108.35 (17) |
O1_1—C10_1—H10A_1 | 109.8 | O1_2—C10_2—H10A_2 | 110.0 |
C9_1—C10_1—H10A_1 | 109.8 | C9_2—C10_2—H10A_2 | 110.0 |
O1_1—C10_1—H10B_1 | 109.8 | O1_2—C10_2—H10B_2 | 110.0 |
C9_1—C10_1—H10B_1 | 109.8 | C9_2—C10_2—H10B_2 | 110.0 |
H10A_1—C10_1—H10B_1 | 108.3 | H10A_2—C10_2—H10B_2 | 108.4 |
C1_1—O1_1—C10_1 | 114.19 (17) | C10_2—O1_2—C1_2 | 114.42 (16) |
C3_1—O2_1—C2_1 | 113.35 (16) | C2_2—O2_2—C3_2 | 113.79 (16) |
C7_1—O4_1—C6_1 | 111.98 (16) | C4_2—O3_2—C5_2 | 113.74 (17) |
C5_1—O3_1—C4_1 | 115.00 (16) | C7_2—O4_2—C6_2 | 112.89 (16) |
C9_1—O5_1—C8_1 | 114.57 (17) | C8_2—O5_2—C9_2 | 114.65 (16) |
O7_1—Ni1_1—O6_1 | 178.31 (7) | O6_2—Ni2_2—O11_2 | 91.14 (6) |
O7_1—Ni1_1—O9_1 | 92.91 (6) | O6_2—Ni2_2—O7_2 | 174.84 (7) |
O6_1—Ni1_1—O9_1 | 86.54 (6) | O11_2—Ni2_2—O7_2 | 93.92 (6) |
O7_1—Ni1_1—O11_1 | 88.89 (6) | O6_2—Ni2_2—O8_2 | 88.14 (6) |
O6_1—Ni1_1—O11_1 | 91.68 (6) | O11_2—Ni2_2—O8_2 | 88.96 (7) |
O9_1—Ni1_1—O11_1 | 178.10 (6) | O7_2—Ni2_2—O8_2 | 92.99 (6) |
O7_1—Ni1_1—O8_1 | 90.25 (6) | O6_2—Ni2_2—O9_2 | 88.29 (6) |
O6_1—Ni1_1—O8_1 | 91.39 (6) | O11_2—Ni2_2—O9_2 | 174.67 (6) |
O9_1—Ni1_1—O8_1 | 94.14 (6) | O7_2—Ni2_2—O9_2 | 86.58 (6) |
O11_1—Ni1_1—O8_1 | 85.24 (6) | O8_2—Ni2_2—O9_2 | 96.32 (6) |
O7_1—Ni1_1—O10_1 | 90.74 (6) | O6_2—Ni2_2—O10_2 | 89.46 (6) |
O6_1—Ni1_1—O10_1 | 87.72 (6) | O11_2—Ni2_2—O10_2 | 94.54 (6) |
O9_1—Ni1_1—O10_1 | 96.03 (6) | O7_2—Ni2_2—O10_2 | 89.09 (6) |
O11_1—Ni1_1—O10_1 | 84.54 (6) | O8_2—Ni2_2—O10_2 | 175.80 (6) |
O8_1—Ni1_1—O10_1 | 169.72 (6) | O9_2—Ni2_2—O10_2 | 80.16 (6) |
Ni1_1—O6_1—H6C_1 | 121.0 (16) | Ni2_2—O6_2—H6C_2 | 123.1 (16) |
Ni1_1—O6_1—H6D_1 | 119.8 (16) | Ni2_2—O6_2—H6D_2 | 114.2 (16) |
H6C_1—O6_1—H6D_1 | 110 (2) | H6C_2—O6_2—H6D_2 | 107.2 (19) |
Ni1_1—O7_1—H7C_1 | 121.2 (16) | Ni2_2—O7_2—H7C_2 | 129.7 (16) |
Ni1_1—O7_1—H7D_1 | 117.2 (16) | Ni2_2—O7_2—H7D_2 | 116.3 (16) |
H7C_1—O7_1—H7D_1 | 108.0 (19) | H7C_2—O7_2—H7D_2 | 109.4 (19) |
Ni1_1—O9_1—H9C_1 | 115.8 (17) | Ni2_2—O8_2—H8C_2 | 101.7 (17) |
Ni1_1—O9_1—H9D_1 | 101.5 (16) | Ni2_2—O8_2—H8D_2 | 111.7 (17) |
H9C_1—O9_1—H9D_1 | 105.7 (19) | H8C_2—O8_2—H8D_2 | 107.1 (19) |
Ni1_1—O11_1—H11C_1 | 115.1 (16) | Ni2_2—O11_2—H11C_2 | 116.7 (16) |
Ni1_1—O11_1—H11D_1 | 109.6 (16) | Ni2_2—O11_2—H11D_2 | 104.5 (18) |
H11C_1—O11_1—H11D_1 | 103.5 (18) | H11C_2—O11_2—H11D_2 | 106.9 (19) |
O12_1—N1_1—O13_1 | 122.23 (18) | O12_2—N1_2—O13_2 | 120.47 (18) |
O12_1—N1_1—O10_1 | 120.63 (18) | O12_2—N1_2—O10_2 | 118.72 (18) |
O13_1—N1_1—O10_1 | 117.14 (18) | O13_2—N1_2—O10_2 | 120.81 (18) |
N1_1—O10_1—Ni1_1 | 127.24 (13) | N1_2—O10_2—Ni2_2 | 130.04 (14) |
O15_1—N2_1—O14_1 | 121.65 (19) | O14_2—N2_2—O15_2 | 120.66 (18) |
O15_1—N2_1—O8_1 | 118.79 (19) | O14_2—N2_2—O9_2 | 118.75 (19) |
O14_1—N2_1—O8_1 | 119.56 (19) | O15_2—N2_2—O9_2 | 120.60 (18) |
N2_1—O8_1—Ni1_1 | 128.91 (14) | N2_2—O9_2—Ni2_2 | 128.20 (13) |
| | | |
O1_1—C1_1—C2_1—O2_1 | 67.2 (2) | O10_1—Ni1_1—O8_1—N2_1 | −143.6 (3) |
O2_1—C3_1—C4_1—O3_1 | −62.2 (2) | O1_2—C1_2—C2_2—O2_2 | −65.5 (2) |
O3_1—C5_1—C6_1—O4_1 | 64.0 (2) | O2_2—C3_2—C4_2—O3_2 | 66.1 (2) |
O4_1—C7_1—C8_1—O5_1 | −57.5 (2) | O3_2—C5_2—C6_2—O4_2 | −66.4 (2) |
O5_1—C9_1—C10_1—O1_1 | −73.0 (2) | O4_2—C7_2—C8_2—O5_2 | 58.8 (2) |
C2_1—C1_1—O1_1—C10_1 | −177.60 (18) | O5_2—C9_2—C10_2—O1_2 | 69.4 (2) |
C9_1—C10_1—O1_1—C1_1 | 153.14 (18) | C9_2—C10_2—O1_2—C1_2 | −155.74 (17) |
C4_1—C3_1—O2_1—C2_1 | 164.74 (18) | C2_2—C1_2—O1_2—C10_2 | −177.10 (17) |
C1_1—C2_1—O2_1—C3_1 | −161.34 (18) | C1_2—C2_2—O2_2—C3_2 | 154.95 (18) |
C8_1—C7_1—O4_1—C6_1 | −178.13 (18) | C4_2—C3_2—O2_2—C2_2 | −161.26 (18) |
C5_1—C6_1—O4_1—C7_1 | −163.88 (18) | C3_2—C4_2—O3_2—C5_2 | −172.22 (17) |
C6_1—C5_1—O3_1—C4_1 | −168.75 (17) | C6_2—C5_2—O3_2—C4_2 | 170.00 (17) |
C3_1—C4_1—O3_1—C5_1 | 171.62 (16) | C8_2—C7_2—O4_2—C6_2 | −178.73 (17) |
C10_1—C9_1—O5_1—C8_1 | 174.72 (17) | C5_2—C6_2—O4_2—C7_2 | 162.84 (18) |
C7_1—C8_1—O5_1—C9_1 | −85.8 (2) | C7_2—C8_2—O5_2—C9_2 | 83.0 (2) |
O12_1—N1_1—O10_1—Ni1_1 | −17.8 (3) | C10_2—C9_2—O5_2—C8_2 | −175.97 (17) |
O13_1—N1_1—O10_1—Ni1_1 | 162.49 (13) | O12_2—N1_2—O10_2—Ni2_2 | 172.34 (13) |
O7_1—Ni1_1—O10_1—N1_1 | −45.39 (16) | O13_2—N1_2—O10_2—Ni2_2 | −7.9 (3) |
O6_1—Ni1_1—O10_1—N1_1 | 133.88 (16) | O6_2—Ni2_2—O10_2—N1_2 | −93.83 (16) |
O9_1—Ni1_1—O10_1—N1_1 | 47.61 (16) | O11_2—Ni2_2—O10_2—N1_2 | −2.74 (16) |
O11_1—Ni1_1—O10_1—N1_1 | −134.21 (16) | O7_2—Ni2_2—O10_2—N1_2 | 91.13 (16) |
O8_1—Ni1_1—O10_1—N1_1 | −140.9 (3) | O9_2—Ni2_2—O10_2—N1_2 | 177.81 (16) |
O15_1—N2_1—O8_1—Ni1_1 | 163.60 (14) | O14_2—N2_2—O9_2—Ni2_2 | 168.68 (14) |
O14_1—N2_1—O8_1—Ni1_1 | −16.5 (3) | O15_2—N2_2—O9_2—Ni2_2 | −11.0 (3) |
O7_1—Ni1_1—O8_1—N2_1 | 120.88 (17) | O6_2—Ni2_2—O9_2—N2_2 | 105.75 (16) |
O6_1—Ni1_1—O8_1—N2_1 | −58.68 (17) | O7_2—Ni2_2—O9_2—N2_2 | −74.82 (16) |
O9_1—Ni1_1—O8_1—N2_1 | 27.94 (17) | O8_2—Ni2_2—O9_2—N2_2 | 17.81 (16) |
O11_1—Ni1_1—O8_1—N2_1 | −150.26 (17) | O10_2—Ni2_2—O9_2—N2_2 | −164.50 (16) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O6_1—H6C_1···O2_2 | 0.81 (2) | 2.02 (2) | 2.823 (2) | 171 (2) |
O6_1—H6D_1···O4_2 | 0.81 (2) | 2.07 (2) | 2.868 (2) | 169 (2) |
O7_1—H7C_1···O2_1 | 0.81 (2) | 2.00 (2) | 2.772 (2) | 159 (2) |
O7_1—H7D_1···O4_1 | 0.83 (2) | 1.99 (2) | 2.809 (2) | 170 (2) |
O9_1—H9C_1···O12_2i | 0.81 (2) | 2.15 (2) | 2.868 (2) | 149 (2) |
O9_1—H9D_1···O14_1 | 0.84 (2) | 1.91 (2) | 2.707 (2) | 157 (2) |
O11_1—H11C_1···O5_1 | 0.83 (2) | 1.91 (2) | 2.733 (2) | 174 (2) |
O11_1—H11D_1···O5_2 | 0.84 (2) | 1.85 (2) | 2.687 (2) | 169 (2) |
O6_2—H6C_2···O1_1ii | 0.82 (2) | 1.99 (2) | 2.780 (2) | 161 (2) |
O6_2—H6D_2···O3_1ii | 0.84 (2) | 1.84 (2) | 2.675 (2) | 174 (2) |
O7_2—H7C_2···O1_2 | 0.83 (2) | 1.89 (2) | 2.702 (2) | 165 (2) |
O7_2—H7D_2···O3_2 | 0.81 (2) | 1.95 (2) | 2.754 (2) | 176 (2) |
O8_2—H8C_2···O15_2 | 0.84 (2) | 1.90 (2) | 2.679 (2) | 155 (2) |
O8_2—H8D_2···O12_1iii | 0.83 (2) | 1.98 (2) | 2.805 (2) | 172 (2) |
O11_2—H11C_2···O13_1iii | 0.84 (2) | 1.87 (2) | 2.709 (2) | 179 (3) |
O11_2—H11D_2···O13_2 | 0.82 (2) | 1.94 (2) | 2.700 (2) | 156 (2) |
Symmetry codes: (i) −x+1, y−1/2, −z+1/2; (ii) x, −y+1/2, z+1/2; (iii) x−1/2, y, −z+1/2. |
Crystal data top
C10H20O5·C2H7N3NiO8·C2H3N | Z = 4 |
Mr = 521.13 | F(000) = 1096 |
Triclinic, P1 | Dx = 1.519 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 12.144 (1) Å | Cell parameters from 9946 reflections |
b = 12.137 (1) Å | θ = 1.0–27.5° |
c = 16.039 (1) Å | µ = 0.92 mm−1 |
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 tube | 7375 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.051 |
Detector resolution: 18 pixels mm-1 | θmax = 27.5°, θmin = 1.3° |
ω scans at fixed χ = 55° | h = −15→15 |
Absorption correction: multi-scan Scalepack (Otwinowski & Minor, 2006) | k = −15→15 |
Tmin = 0.837, Tmax = 0.930 | l = −20→20 |
19489 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.095 | H 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 parameters | Δρmax = 0.77 e Å−3 |
12 restraints | Δρmin = −0.57 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
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 | x | y | z | Uiso*/Ueq | |
C1_1 | 0.0603 (3) | 0.1550 (3) | 0.3048 (3) | 0.0239 (10) | |
H1A_1 | 0.0622 | 0.1688 | 0.2443 | 0.029* | |
H1B_1 | −0.0196 | 0.1394 | 0.3051 | 0.029* | |
C2_1 | 0.1352 (3) | 0.0590 (4) | 0.3411 (3) | 0.0242 (11) | |
H2A_1 | 0.1343 | 0.0456 | 0.4017 | 0.029* | |
H2B_1 | 0.1078 | −0.0083 | 0.3068 | 0.029* | |
C3_1 | 0.3322 (3) | 0.0048 (3) | 0.3745 (3) | 0.0250 (10) | |
H3A_1 | 0.3222 | −0.0611 | 0.3368 | 0.030* | |
H3B_1 | 0.3231 | −0.0177 | 0.4316 | 0.030* | |
C4_1 | 0.4484 (3) | 0.0530 (3) | 0.3849 (3) | 0.0211 (10) | |
H4A_1 | 0.5068 | −0.0059 | 0.3989 | 0.025* | |
H4B_1 | 0.4526 | 0.0885 | 0.3303 | 0.025* | |
C5_1 | 0.5705 (3) | 0.1978 (3) | 0.4632 (2) | 0.0194 (9) | |
H5A_1 | 0.6282 | 0.1537 | 0.4443 | 0.023* | |
H5B_1 | 0.6026 | 0.2163 | 0.5251 | 0.023* | |
C6_1 | 0.5479 (3) | 0.3024 (3) | 0.4115 (2) | 0.0198 (9) | |
H6A_1 | 0.6191 | 0.3459 | 0.4204 | 0.024* | |
H6B_1 | 0.5188 | 0.2853 | 0.3491 | 0.024* | |
C7_1 | 0.4349 (3) | 0.4646 (3) | 0.3965 (3) | 0.0214 (10) | |
H7A_1 | 0.4283 | 0.4555 | 0.3340 | 0.026* | |
H7B_1 | 0.4940 | 0.5211 | 0.4201 | 0.026* | |
C8_1 | 0.3226 (3) | 0.4990 (3) | 0.4101 (2) | 0.0219 (10) | |
H8A_1 | 0.3211 | 0.4837 | 0.4704 | 0.026* | |
H8B_1 | 0.3108 | 0.5790 | 0.3994 | 0.026* | |
C9_1 | 0.1248 (3) | 0.4424 (4) | 0.3682 (3) | 0.0225 (11) | |
H9A_1 | 0.0877 | 0.5141 | 0.3494 | 0.027* | |
H9B_1 | 0.1330 | 0.4339 | 0.4310 | 0.027* | |
C10_1 | 0.0546 (3) | 0.3509 (3) | 0.3192 (3) | 0.0218 (10) | |
H10A_1 | −0.0256 | 0.3577 | 0.3220 | 0.026* | |
H10B_1 | 0.0558 | 0.3531 | 0.2578 | 0.026* | |
O1_1 | 0.10252 (19) | 0.2501 (2) | 0.35782 (15) | 0.0199 (6) | |
O2_1 | 0.2488 (2) | 0.0858 (2) | 0.33695 (17) | 0.0187 (6) | |
O3_1 | 0.4696 (2) | 0.1332 (2) | 0.45365 (16) | 0.0198 (6) | |
O4_1 | 0.4652 (2) | 0.3627 (2) | 0.44052 (17) | 0.0203 (7) | |
O5_1 | 0.2342 (2) | 0.4378 (2) | 0.35084 (17) | 0.0217 (7) | |
Ni1_1 | 0.30366 (4) | 0.26565 (4) | 0.13580 (3) | 0.01610 (12) | |
O6_1 | 0.3049 (2) | 0.2687 (2) | 0.26255 (16) | 0.0164 (6) | |
H6C_1 | 0.291 (3) | 0.2058 (15) | 0.277 (2) | 0.025* | |
H6D_1 | 0.270 (3) | 0.311 (2) | 0.289 (2) | 0.025* | |
O7_1 | 0.29221 (19) | 0.2614 (3) | 0.00815 (15) | 0.0261 (7) | |
H7C_1 | 0.3478 (18) | 0.271 (3) | −0.011 (2) | 0.039* | |
H7D_1 | 0.2352 (18) | 0.252 (4) | −0.0330 (17) | 0.039* | |
N1_1 | 0.2200 (3) | 0.0417 (3) | 0.1387 (2) | 0.0255 (9) | |
O8_1 | 0.3104 (2) | 0.0977 (2) | 0.14659 (16) | 0.0248 (6) | |
O9_1 | 0.1251 (2) | 0.0865 (2) | 0.11432 (16) | 0.0348 (7) | |
O10_1 | 0.2264 (2) | −0.0576 (2) | 0.15822 (17) | 0.0331 (7) | |
N2_1 | 0.1861 (3) | 0.4366 (3) | 0.1186 (2) | 0.0274 (9) | |
O11_1 | 0.2950 (2) | 0.4387 (2) | 0.13714 (19) | 0.0219 (6) | |
O12_1 | 0.1393 (2) | 0.3419 (2) | 0.10731 (18) | 0.0253 (7) | |
O13_1 | 0.1297 (3) | 0.5217 (3) | 0.1125 (2) | 0.0448 (9) | |
C11_1 | 0.6921 (3) | 0.2426 (4) | 0.2551 (2) | 0.0259 (9) | |
H11A_1 | 0.7124 | 0.3073 | 0.2928 | 0.039* | |
H11B_1 | 0.7408 | 0.2397 | 0.2153 | 0.039* | |
H11C_1 | 0.7034 | 0.1757 | 0.2905 | 0.039* | |
C12_1 | 0.5723 (3) | 0.2501 (3) | 0.2056 (2) | 0.0192 (8) | |
N3_1 | 0.4793 (2) | 0.2570 (3) | 0.16895 (18) | 0.0215 (8) | |
C13_1 | −0.0698 (3) | 0.2318 (4) | −0.0145 (2) | 0.0296 (10) | |
H13A_1 | 0.0073 | 0.2012 | 0.0062 | 0.044* | |
H13B_1 | −0.0668 | 0.3003 | −0.0461 | 0.044* | |
H13C_1 | −0.1193 | 0.1785 | −0.0531 | 0.044* | |
C14_1 | −0.1152 (3) | 0.2546 (4) | 0.0586 (3) | 0.0225 (9) | |
N4_1 | −0.1527 (3) | 0.2706 (3) | 0.1160 (2) | 0.0295 (9) | |
C1_2 | 0.0642 (3) | 0.3380 (3) | 0.8083 (3) | 0.0215 (10) | |
H1A_2 | −0.0162 | 0.3536 | 0.8070 | 0.026* | |
H1B_2 | 0.0686 | 0.3253 | 0.7483 | 0.026* | |
C2_2 | 0.1396 (3) | 0.4331 (4) | 0.8482 (3) | 0.0231 (10) | |
H2A_2 | 0.1130 | 0.5018 | 0.8158 | 0.028* | |
H2B_2 | 0.1377 | 0.4438 | 0.9090 | 0.028* | |
C3_2 | 0.3376 (3) | 0.4858 (3) | 0.8853 (3) | 0.0235 (10) | |
H3A_2 | 0.3301 | 0.5034 | 0.9438 | 0.028* | |
H3B_2 | 0.3273 | 0.5547 | 0.8511 | 0.028* | |
C4_2 | 0.4537 (3) | 0.4383 (3) | 0.8917 (3) | 0.0199 (10) | |
H4A_2 | 0.4555 | 0.4040 | 0.8360 | 0.024* | |
H4B_2 | 0.5125 | 0.4970 | 0.9056 | 0.024* | |
C5_2 | 0.5761 (3) | 0.2929 (3) | 0.9633 (2) | 0.0213 (9) | |
H5A_2 | 0.6110 | 0.2715 | 1.0241 | 0.026* | |
H5B_2 | 0.6323 | 0.3383 | 0.9439 | 0.026* | |
C6_2 | 0.5499 (3) | 0.1906 (3) | 0.9081 (2) | 0.0210 (10) | |
H6A_2 | 0.5189 | 0.2107 | 0.8465 | 0.025* | |
H6B_2 | 0.6203 | 0.1468 | 0.9139 | 0.025* | |
C7_2 | 0.4366 (3) | 0.0271 (3) | 0.8916 (3) | 0.0203 (10) | |
H7A_2 | 0.4954 | −0.0297 | 0.9141 | 0.024* | |
H7B_2 | 0.4297 | 0.0374 | 0.8292 | 0.024* | |
C8_2 | 0.3237 (3) | −0.0084 (4) | 0.9048 (3) | 0.0230 (10) | |
H8A_2 | 0.3102 | −0.0874 | 0.8902 | 0.028* | |
H8B_2 | 0.3236 | 0.0025 | 0.9659 | 0.028* | |
C9_2 | 0.1281 (3) | 0.0491 (4) | 0.8680 (3) | 0.0232 (11) | |
H9A_2 | 0.1373 | 0.0558 | 0.9310 | 0.028* | |
H9B_2 | 0.0919 | −0.0228 | 0.8482 | 0.028* | |
C10_2 | 0.0553 (3) | 0.1420 (3) | 0.8205 (3) | 0.0204 (10) | |
H10A_2 | 0.0545 | 0.1409 | 0.7586 | 0.024* | |
H10B_2 | −0.0242 | 0.1342 | 0.8247 | 0.024* | |
O1_2 | 0.10401 (19) | 0.2437 (2) | 0.86012 (15) | 0.0200 (6) | |
O2_2 | 0.2525 (2) | 0.4073 (2) | 0.84435 (17) | 0.0201 (7) | |
O3_2 | 0.4759 (2) | 0.3573 (2) | 0.95883 (17) | 0.0190 (6) | |
O4_2 | 0.4682 (2) | 0.1287 (2) | 0.93722 (17) | 0.0194 (7) | |
O5_2 | 0.2366 (2) | 0.0568 (2) | 0.84958 (17) | 0.0203 (7) | |
Ni2_2 | 0.29650 (4) | 0.22252 (4) | 0.63415 (3) | 0.01618 (13) | |
O6_2 | 0.3031 (2) | 0.2275 (2) | 0.76117 (16) | 0.0177 (6) | |
H6C_2 | 0.284 (3) | 0.1746 (18) | 0.788 (2) | 0.027* | |
H6D_2 | 0.280 (3) | 0.2836 (17) | 0.782 (2) | 0.027* | |
O7_2 | 0.2865 (2) | 0.2124 (2) | 0.50680 (15) | 0.0233 (7) | |
H7C_2 | 0.3446 (18) | 0.203 (3) | 0.4869 (19) | 0.035* | |
H7D_2 | 0.2340 (19) | 0.230 (3) | 0.4645 (17) | 0.035* | |
N1_2 | 0.2457 (3) | 0.4595 (3) | 0.6422 (2) | 0.0234 (8) | |
O8_2 | 0.3473 (2) | 0.4709 (2) | 0.68356 (16) | 0.0288 (6) | |
O9_2 | 0.2086 (2) | 0.3632 (2) | 0.61173 (15) | 0.0269 (6) | |
O10_2 | 0.1796 (3) | 0.5369 (2) | 0.6298 (2) | 0.0477 (9) | |
N2_2 | 0.1993 (3) | 0.0374 (3) | 0.6218 (2) | 0.0251 (9) | |
O11_2 | 0.3085 (2) | 0.0488 (2) | 0.64360 (18) | 0.0202 (6) | |
O12_2 | 0.1437 (2) | 0.1273 (2) | 0.61016 (16) | 0.0204 (6) | |
O13_2 | 0.1538 (2) | −0.0523 (2) | 0.6131 (2) | 0.0414 (8) | |
C11_2 | 0.6786 (3) | 0.2953 (3) | 0.7514 (2) | 0.0245 (10) | |
H11A_2 | 0.6831 | 0.3679 | 0.7790 | 0.037* | |
H11B_2 | 0.7289 | 0.2936 | 0.7128 | 0.037* | |
H11C_2 | 0.7025 | 0.2386 | 0.7960 | 0.037* | |
C12_2 | 0.5620 (3) | 0.2742 (3) | 0.7019 (2) | 0.0202 (9) | |
N3_2 | 0.4685 (2) | 0.2567 (3) | 0.66560 (18) | 0.0198 (7) | |
C13_2 | −0.0517 (3) | 0.2723 (4) | 0.4996 (3) | 0.0326 (11) | |
H13A_2 | −0.1039 | 0.3084 | 0.4500 | 0.049* | |
H13B_2 | −0.0251 | 0.2026 | 0.4808 | 0.049* | |
H13C_2 | 0.0140 | 0.3204 | 0.5235 | 0.049* | |
C14_2 | −0.1112 (3) | 0.2504 (4) | 0.5658 (3) | 0.0237 (9) | |
N4_2 | −0.1583 (3) | 0.2349 (3) | 0.6170 (2) | 0.0335 (9) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1_1 | 0.019 (2) | 0.031 (3) | 0.020 (3) | −0.0003 (19) | 0.0014 (19) | −0.004 (2) |
C2_1 | 0.021 (2) | 0.031 (3) | 0.024 (3) | −0.010 (2) | 0.0112 (19) | −0.005 (2) |
C3_1 | 0.032 (3) | 0.018 (2) | 0.022 (2) | 0.0073 (19) | 0.0022 (19) | 0.0013 (18) |
C4_1 | 0.025 (2) | 0.018 (2) | 0.021 (2) | 0.0107 (19) | 0.0059 (18) | 0.0011 (19) |
C5_1 | 0.0122 (19) | 0.030 (2) | 0.015 (2) | 0.0044 (17) | 0.0024 (16) | 0.0043 (19) |
C6_1 | 0.017 (2) | 0.029 (3) | 0.014 (2) | −0.0013 (18) | 0.0061 (17) | 0.0002 (19) |
C7_1 | 0.026 (2) | 0.024 (2) | 0.013 (2) | −0.0015 (19) | 0.0039 (19) | 0.0007 (19) |
C8_1 | 0.027 (2) | 0.020 (2) | 0.018 (2) | 0.0013 (18) | 0.0043 (19) | −0.0071 (18) |
C9_1 | 0.023 (2) | 0.029 (3) | 0.020 (2) | 0.010 (2) | 0.0119 (19) | 0.008 (2) |
C10_1 | 0.014 (2) | 0.029 (3) | 0.021 (3) | 0.0040 (19) | 0.0015 (19) | 0.003 (2) |
O1_1 | 0.0165 (13) | 0.0242 (17) | 0.0176 (16) | 0.0039 (14) | 0.0024 (11) | 0.0010 (15) |
O2_1 | 0.0169 (14) | 0.0178 (15) | 0.0219 (16) | 0.0018 (12) | 0.0061 (12) | 0.0049 (12) |
O3_1 | 0.0220 (15) | 0.0231 (16) | 0.0151 (15) | −0.0051 (12) | 0.0062 (12) | −0.0028 (12) |
O4_1 | 0.0197 (15) | 0.0217 (16) | 0.0203 (16) | 0.0031 (13) | 0.0069 (13) | 0.0013 (13) |
O5_1 | 0.0177 (15) | 0.0317 (18) | 0.0157 (16) | 0.0012 (13) | 0.0048 (12) | −0.0037 (14) |
Ni1_1 | 0.0146 (2) | 0.0215 (3) | 0.0128 (3) | −0.0019 (2) | 0.0048 (2) | −0.0002 (2) |
O6_1 | 0.0230 (13) | 0.0126 (15) | 0.0155 (15) | 0.0026 (13) | 0.0085 (11) | 0.0001 (13) |
O7_1 | 0.0145 (12) | 0.054 (2) | 0.0107 (14) | −0.0032 (14) | 0.0050 (10) | 0.0007 (14) |
N1_1 | 0.028 (2) | 0.035 (2) | 0.016 (2) | −0.0002 (18) | 0.0108 (16) | −0.0050 (17) |
O8_1 | 0.0267 (15) | 0.0217 (14) | 0.0306 (15) | −0.0081 (13) | 0.0160 (12) | −0.0066 (12) |
O9_1 | 0.0260 (15) | 0.0390 (18) | 0.0368 (16) | 0.0058 (14) | 0.0037 (13) | 0.0029 (14) |
O10_1 | 0.0417 (18) | 0.0198 (17) | 0.0428 (18) | −0.0043 (14) | 0.0200 (15) | 0.0001 (14) |
N2_1 | 0.024 (2) | 0.038 (3) | 0.0211 (19) | 0.0114 (18) | 0.0065 (16) | −0.0007 (17) |
O11_1 | 0.0191 (14) | 0.0203 (14) | 0.0273 (16) | −0.0002 (13) | 0.0078 (12) | 0.0040 (14) |
O12_1 | 0.0190 (15) | 0.0282 (17) | 0.0285 (16) | −0.0049 (12) | 0.0058 (12) | −0.0055 (13) |
O13_1 | 0.0424 (19) | 0.040 (2) | 0.047 (2) | 0.0226 (17) | 0.0040 (16) | −0.0013 (16) |
C11_1 | 0.0189 (18) | 0.038 (3) | 0.021 (2) | 0.0018 (18) | 0.0059 (15) | 0.0012 (19) |
C12_1 | 0.0247 (19) | 0.023 (2) | 0.0132 (19) | −0.0019 (18) | 0.0103 (16) | 0.0004 (17) |
N3_1 | 0.0206 (16) | 0.031 (2) | 0.0136 (17) | −0.0002 (17) | 0.0062 (13) | −0.0001 (17) |
C13_1 | 0.029 (2) | 0.035 (3) | 0.026 (2) | −0.002 (2) | 0.0101 (18) | −0.004 (2) |
C14_1 | 0.0122 (18) | 0.024 (2) | 0.029 (2) | −0.0017 (19) | 0.0012 (17) | 0.003 (2) |
N4_1 | 0.0238 (18) | 0.037 (2) | 0.030 (2) | −0.0024 (18) | 0.0111 (16) | 0.0018 (19) |
C1_2 | 0.015 (2) | 0.028 (2) | 0.020 (2) | 0.0038 (18) | 0.0029 (19) | −0.001 (2) |
C2_2 | 0.018 (2) | 0.023 (3) | 0.026 (3) | 0.0062 (19) | 0.0018 (19) | −0.001 (2) |
C3_2 | 0.019 (2) | 0.021 (2) | 0.029 (2) | −0.0021 (18) | 0.0040 (19) | −0.0026 (19) |
C4_2 | 0.017 (2) | 0.023 (2) | 0.019 (2) | 0.0019 (18) | 0.0040 (18) | 0.0028 (19) |
C5_2 | 0.0157 (19) | 0.028 (2) | 0.021 (2) | 0.0022 (18) | 0.0062 (17) | 0.0058 (19) |
C6_2 | 0.019 (2) | 0.026 (2) | 0.018 (2) | 0.0009 (18) | 0.0045 (17) | 0.0029 (19) |
C7_2 | 0.020 (2) | 0.017 (2) | 0.023 (2) | −0.0001 (18) | 0.0046 (18) | −0.0013 (19) |
C8_2 | 0.024 (2) | 0.020 (2) | 0.021 (2) | 0.0024 (18) | −0.0015 (19) | 0.0022 (18) |
C9_2 | 0.021 (2) | 0.026 (3) | 0.024 (3) | −0.004 (2) | 0.009 (2) | 0.007 (2) |
C10_2 | 0.016 (2) | 0.026 (2) | 0.021 (2) | −0.0075 (18) | 0.0077 (19) | −0.006 (2) |
O1_2 | 0.0185 (13) | 0.0242 (17) | 0.0146 (15) | −0.0018 (14) | −0.0002 (11) | 0.0002 (14) |
O2_2 | 0.0157 (15) | 0.0227 (16) | 0.0219 (16) | −0.0027 (12) | 0.0052 (12) | −0.0023 (13) |
O3_2 | 0.0165 (14) | 0.0210 (15) | 0.0216 (16) | 0.0003 (12) | 0.0090 (12) | 0.0009 (13) |
O4_2 | 0.0216 (15) | 0.0225 (16) | 0.0159 (16) | −0.0025 (13) | 0.0081 (12) | −0.0015 (13) |
O5_2 | 0.0174 (15) | 0.0238 (17) | 0.0211 (17) | 0.0013 (13) | 0.0073 (12) | 0.0062 (14) |
Ni2_2 | 0.0153 (2) | 0.0209 (3) | 0.0126 (3) | 0.0020 (2) | 0.0042 (2) | 0.0003 (2) |
O6_2 | 0.0217 (13) | 0.0210 (16) | 0.0127 (15) | 0.0032 (13) | 0.0084 (11) | 0.0013 (13) |
O7_2 | 0.0179 (13) | 0.0418 (19) | 0.0109 (14) | 0.0070 (13) | 0.0050 (11) | 0.0012 (13) |
N1_2 | 0.031 (2) | 0.021 (2) | 0.0154 (19) | −0.0007 (16) | 0.0022 (16) | −0.0006 (15) |
O8_2 | 0.0211 (14) | 0.0273 (16) | 0.0358 (16) | −0.0031 (12) | 0.0036 (12) | −0.0031 (13) |
O9_2 | 0.0319 (16) | 0.0204 (16) | 0.0245 (14) | −0.0003 (12) | 0.0006 (12) | −0.0009 (12) |
O10_2 | 0.0400 (19) | 0.0223 (18) | 0.073 (2) | 0.0163 (15) | 0.0013 (16) | −0.0021 (16) |
N2_2 | 0.025 (2) | 0.028 (2) | 0.0221 (19) | 0.0007 (16) | 0.0063 (16) | 0.0006 (16) |
O11_2 | 0.0137 (13) | 0.0222 (15) | 0.0244 (16) | 0.0033 (12) | 0.0042 (12) | 0.0009 (13) |
O12_2 | 0.0138 (14) | 0.0245 (16) | 0.0213 (15) | 0.0012 (12) | 0.0021 (12) | 0.0021 (13) |
O13_2 | 0.0398 (18) | 0.0251 (18) | 0.055 (2) | −0.0186 (15) | 0.0055 (15) | 0.0027 (16) |
C11_2 | 0.0179 (18) | 0.035 (3) | 0.021 (2) | −0.0015 (17) | 0.0054 (16) | 0.0027 (18) |
C12_2 | 0.0219 (19) | 0.023 (2) | 0.018 (2) | −0.0033 (18) | 0.0102 (16) | 0.0021 (18) |
N3_2 | 0.0234 (16) | 0.0237 (19) | 0.0148 (17) | −0.0015 (16) | 0.0095 (13) | −0.0010 (16) |
C13_2 | 0.024 (2) | 0.045 (3) | 0.030 (2) | 0.003 (2) | 0.0080 (18) | 0.009 (2) |
C14_2 | 0.022 (2) | 0.023 (2) | 0.023 (2) | 0.002 (2) | 0.0004 (18) | −0.001 (2) |
N4_2 | 0.031 (2) | 0.033 (2) | 0.037 (2) | −0.0022 (18) | 0.0111 (17) | −0.001 (2) |
Geometric parameters (Å, º) top
C1_1—O1_1 | 1.442 (5) | C1_2—O1_2 | 1.423 (5) |
C1_1—C2_1 | 1.499 (6) | C1_2—C2_2 | 1.504 (6) |
C1_1—H1A_1 | 0.9900 | C1_2—H1A_2 | 0.9900 |
C1_1—H1B_1 | 0.9900 | C1_2—H1B_2 | 0.9900 |
C2_1—O2_1 | 1.435 (4) | C2_2—O2_2 | 1.425 (4) |
C2_1—H2A_1 | 0.9900 | C2_2—H2A_2 | 0.9900 |
C2_1—H2B_1 | 0.9900 | C2_2—H2B_2 | 0.9900 |
C3_1—O2_1 | 1.426 (4) | C3_2—O2_2 | 1.429 (4) |
C3_1—C4_1 | 1.495 (5) | C3_2—C4_2 | 1.502 (5) |
C3_1—H3A_1 | 0.9900 | C3_2—H3A_2 | 0.9900 |
C3_1—H3B_1 | 0.9900 | C3_2—H3B_2 | 0.9900 |
C4_1—O3_1 | 1.440 (4) | C4_2—O3_2 | 1.432 (4) |
C4_1—H4A_1 | 0.9900 | C4_2—H4A_2 | 0.9900 |
C4_1—H4B_1 | 0.9900 | C4_2—H4B_2 | 0.9900 |
C5_1—O3_1 | 1.427 (4) | C5_2—O3_2 | 1.432 (4) |
C5_1—C6_1 | 1.503 (5) | C5_2—C6_2 | 1.507 (5) |
C5_1—H5A_1 | 0.9900 | C5_2—H5A_2 | 0.9900 |
C5_1—H5B_1 | 0.9900 | C5_2—H5B_2 | 0.9900 |
C6_1—O4_1 | 1.418 (4) | C6_2—O4_2 | 1.420 (4) |
C6_1—H6A_1 | 0.9900 | C6_2—H6A_2 | 0.9900 |
C6_1—H6B_1 | 0.9900 | C6_2—H6B_2 | 0.9900 |
C7_1—O4_1 | 1.425 (5) | C7_2—O4_2 | 1.431 (4) |
C7_1—C8_1 | 1.497 (5) | C7_2—C8_2 | 1.505 (5) |
C7_1—H7A_1 | 0.9900 | C7_2—H7A_2 | 0.9900 |
C7_1—H7B_1 | 0.9900 | C7_2—H7B_2 | 0.9900 |
C8_1—O5_1 | 1.435 (4) | C8_2—O5_2 | 1.426 (4) |
C8_1—H8A_1 | 0.9900 | C8_2—H8A_2 | 0.9900 |
C8_1—H8B_1 | 0.9900 | C8_2—H8B_2 | 0.9900 |
C9_1—O5_1 | 1.430 (4) | C9_2—O5_2 | 1.428 (4) |
C9_1—C10_1 | 1.488 (6) | C9_2—C10_2 | 1.510 (6) |
C9_1—H9A_1 | 0.9900 | C9_2—H9A_2 | 0.9900 |
C9_1—H9B_1 | 0.9900 | C9_2—H9B_2 | 0.9900 |
C10_1—O1_1 | 1.425 (5) | C10_2—O1_2 | 1.439 (5) |
C10_1—H10A_1 | 0.9900 | C10_2—H10A_2 | 0.9900 |
C10_1—H10B_1 | 0.9900 | C10_2—H10B_2 | 0.9900 |
Ni1_1—O7_1 | 2.015 (2) | Ni2_2—O9_2 | 1.997 (3) |
Ni1_1—O6_1 | 2.029 (2) | Ni2_2—O7_2 | 2.017 (2) |
Ni1_1—O8_1 | 2.046 (3) | Ni2_2—O6_2 | 2.018 (2) |
Ni1_1—N3_1 | 2.059 (3) | Ni2_2—N3_2 | 2.055 (3) |
Ni1_1—O11_1 | 2.103 (3) | Ni2_2—O11_2 | 2.117 (2) |
Ni1_1—O12_1 | 2.137 (3) | Ni2_2—O12_2 | 2.131 (2) |
O6_1—H6C_1 | 0.832 (17) | O6_2—H6C_2 | 0.840 (17) |
O6_1—H6D_1 | 0.847 (16) | O6_2—H6D_2 | 0.842 (17) |
O7_1—H7C_1 | 0.818 (17) | O7_2—H7C_2 | 0.856 (17) |
O7_1—H7D_1 | 0.828 (17) | O7_2—H7D_2 | 0.825 (17) |
N1_1—O9_1 | 1.241 (4) | N1_2—O10_2 | 1.218 (4) |
N1_1—O10_1 | 1.244 (4) | N1_2—O8_2 | 1.243 (4) |
N1_1—O8_1 | 1.268 (4) | N1_2—O9_2 | 1.298 (4) |
N2_1—O13_1 | 1.230 (4) | N2_2—O13_2 | 1.211 (4) |
N2_1—O12_1 | 1.273 (4) | N2_2—O12_2 | 1.272 (4) |
N2_1—O11_1 | 1.276 (4) | N2_2—O11_2 | 1.284 (4) |
C11_1—C12_1 | 1.462 (5) | C11_2—C12_2 | 1.449 (5) |
C11_1—H11A_1 | 0.9800 | C11_2—H11A_2 | 0.9800 |
C11_1—H11B_1 | 0.9800 | C11_2—H11B_2 | 0.9800 |
C11_1—H11C_1 | 0.9800 | C11_2—H11C_2 | 0.9800 |
C12_1—N3_1 | 1.129 (4) | C12_2—N3_2 | 1.149 (4) |
C13_1—C14_1 | 1.448 (5) | C13_2—C14_2 | 1.460 (5) |
C13_1—H13A_1 | 0.9800 | C13_2—H13A_2 | 0.9800 |
C13_1—H13B_1 | 0.9800 | C13_2—H13B_2 | 0.9800 |
C13_1—H13C_1 | 0.9800 | C13_2—H13C_2 | 0.9800 |
C14_1—N4_1 | 1.147 (4) | C14_2—N4_2 | 1.136 (4) |
| | | |
O1_1—C1_1—C2_1 | 108.0 (3) | O1_2—C1_2—C2_2 | 107.2 (3) |
O1_1—C1_1—H1A_1 | 110.1 | O1_2—C1_2—H1A_2 | 110.3 |
C2_1—C1_1—H1A_1 | 110.1 | C2_2—C1_2—H1A_2 | 110.3 |
O1_1—C1_1—H1B_1 | 110.1 | O1_2—C1_2—H1B_2 | 110.3 |
C2_1—C1_1—H1B_1 | 110.1 | C2_2—C1_2—H1B_2 | 110.3 |
H1A_1—C1_1—H1B_1 | 108.4 | H1A_2—C1_2—H1B_2 | 108.5 |
O2_1—C2_1—C1_1 | 107.3 (3) | O2_2—C2_2—C1_2 | 107.2 (3) |
O2_1—C2_1—H2A_1 | 110.3 | O2_2—C2_2—H2A_2 | 110.3 |
C1_1—C2_1—H2A_1 | 110.3 | C1_2—C2_2—H2A_2 | 110.3 |
O2_1—C2_1—H2B_1 | 110.3 | O2_2—C2_2—H2B_2 | 110.3 |
C1_1—C2_1—H2B_1 | 110.3 | C1_2—C2_2—H2B_2 | 110.3 |
H2A_1—C2_1—H2B_1 | 108.5 | H2A_2—C2_2—H2B_2 | 108.5 |
O2_1—C3_1—C4_1 | 108.7 (3) | O2_2—C3_2—C4_2 | 109.0 (3) |
O2_1—C3_1—H3A_1 | 109.9 | O2_2—C3_2—H3A_2 | 109.9 |
C4_1—C3_1—H3A_1 | 109.9 | C4_2—C3_2—H3A_2 | 109.9 |
O2_1—C3_1—H3B_1 | 109.9 | O2_2—C3_2—H3B_2 | 109.9 |
C4_1—C3_1—H3B_1 | 109.9 | C4_2—C3_2—H3B_2 | 109.9 |
H3A_1—C3_1—H3B_1 | 108.3 | H3A_2—C3_2—H3B_2 | 108.3 |
O3_1—C4_1—C3_1 | 108.6 (3) | O3_2—C4_2—C3_2 | 107.5 (3) |
O3_1—C4_1—H4A_1 | 110.0 | O3_2—C4_2—H4A_2 | 110.2 |
C3_1—C4_1—H4A_1 | 110.0 | C3_2—C4_2—H4A_2 | 110.2 |
O3_1—C4_1—H4B_1 | 110.0 | O3_2—C4_2—H4B_2 | 110.2 |
C3_1—C4_1—H4B_1 | 110.0 | C3_2—C4_2—H4B_2 | 110.2 |
H4A_1—C4_1—H4B_1 | 108.4 | H4A_2—C4_2—H4B_2 | 108.5 |
O3_1—C5_1—C6_1 | 112.3 (3) | O3_2—C5_2—C6_2 | 112.2 (3) |
O3_1—C5_1—H5A_1 | 109.1 | O3_2—C5_2—H5A_2 | 109.2 |
C6_1—C5_1—H5A_1 | 109.1 | C6_2—C5_2—H5A_2 | 109.2 |
O3_1—C5_1—H5B_1 | 109.1 | O3_2—C5_2—H5B_2 | 109.2 |
C6_1—C5_1—H5B_1 | 109.1 | C6_2—C5_2—H5B_2 | 109.2 |
H5A_1—C5_1—H5B_1 | 107.9 | H5A_2—C5_2—H5B_2 | 107.9 |
O4_1—C6_1—C5_1 | 107.2 (3) | O4_2—C6_2—C5_2 | 107.4 (3) |
O4_1—C6_1—H6A_1 | 110.3 | O4_2—C6_2—H6A_2 | 110.2 |
C5_1—C6_1—H6A_1 | 110.3 | C5_2—C6_2—H6A_2 | 110.2 |
O4_1—C6_1—H6B_1 | 110.3 | O4_2—C6_2—H6B_2 | 110.2 |
C5_1—C6_1—H6B_1 | 110.3 | C5_2—C6_2—H6B_2 | 110.2 |
H6A_1—C6_1—H6B_1 | 108.5 | H6A_2—C6_2—H6B_2 | 108.5 |
O4_1—C7_1—C8_1 | 107.2 (3) | O4_2—C7_2—C8_2 | 107.7 (3) |
O4_1—C7_1—H7A_1 | 110.3 | O4_2—C7_2—H7A_2 | 110.2 |
C8_1—C7_1—H7A_1 | 110.3 | C8_2—C7_2—H7A_2 | 110.2 |
O4_1—C7_1—H7B_1 | 110.3 | O4_2—C7_2—H7B_2 | 110.2 |
C8_1—C7_1—H7B_1 | 110.3 | C8_2—C7_2—H7B_2 | 110.2 |
H7A_1—C7_1—H7B_1 | 108.5 | H7A_2—C7_2—H7B_2 | 108.5 |
O5_1—C8_1—C7_1 | 108.0 (3) | O5_2—C8_2—C7_2 | 107.8 (3) |
O5_1—C8_1—H8A_1 | 110.1 | O5_2—C8_2—H8A_2 | 110.1 |
C7_1—C8_1—H8A_1 | 110.1 | C7_2—C8_2—H8A_2 | 110.1 |
O5_1—C8_1—H8B_1 | 110.1 | O5_2—C8_2—H8B_2 | 110.1 |
C7_1—C8_1—H8B_1 | 110.1 | C7_2—C8_2—H8B_2 | 110.1 |
H8A_1—C8_1—H8B_1 | 108.4 | H8A_2—C8_2—H8B_2 | 108.5 |
O5_1—C9_1—C10_1 | 107.4 (3) | O5_2—C9_2—C10_2 | 107.1 (3) |
O5_1—C9_1—H9A_1 | 110.2 | O5_2—C9_2—H9A_2 | 110.3 |
C10_1—C9_1—H9A_1 | 110.2 | C10_2—C9_2—H9A_2 | 110.3 |
O5_1—C9_1—H9B_1 | 110.2 | O5_2—C9_2—H9B_2 | 110.3 |
C10_1—C9_1—H9B_1 | 110.2 | C10_2—C9_2—H9B_2 | 110.3 |
H9A_1—C9_1—H9B_1 | 108.5 | H9A_2—C9_2—H9B_2 | 108.5 |
O1_1—C10_1—C9_1 | 107.6 (3) | O1_2—C10_2—C9_2 | 107.6 (3) |
O1_1—C10_1—H10A_1 | 110.2 | O1_2—C10_2—H10A_2 | 110.2 |
C9_1—C10_1—H10A_1 | 110.2 | C9_2—C10_2—H10A_2 | 110.2 |
O1_1—C10_1—H10B_1 | 110.2 | O1_2—C10_2—H10B_2 | 110.2 |
C9_1—C10_1—H10B_1 | 110.2 | C9_2—C10_2—H10B_2 | 110.2 |
H10A_1—C10_1—H10B_1 | 108.5 | H10A_2—C10_2—H10B_2 | 108.5 |
C10_1—O1_1—C1_1 | 113.0 (3) | C1_2—O1_2—C10_2 | 113.4 (3) |
C3_1—O2_1—C2_1 | 114.1 (3) | C2_2—O2_2—C3_2 | 114.8 (3) |
C5_1—O3_1—C4_1 | 115.2 (3) | C4_2—O3_2—C5_2 | 113.6 (3) |
C6_1—O4_1—C7_1 | 113.4 (3) | C6_2—O4_2—C7_2 | 113.8 (3) |
C9_1—O5_1—C8_1 | 114.9 (3) | C8_2—O5_2—C9_2 | 114.0 (3) |
O7_1—Ni1_1—O6_1 | 176.58 (10) | O9_2—Ni2_2—O7_2 | 89.04 (11) |
O7_1—Ni1_1—O8_1 | 93.05 (12) | O9_2—Ni2_2—O6_2 | 91.93 (10) |
O6_1—Ni1_1—O8_1 | 86.67 (10) | O7_2—Ni2_2—O6_2 | 177.88 (11) |
O7_1—Ni1_1—N3_1 | 92.70 (10) | O9_2—Ni2_2—N3_2 | 109.37 (13) |
O6_1—Ni1_1—N3_1 | 90.67 (11) | O7_2—Ni2_2—N3_2 | 92.47 (10) |
O8_1—Ni1_1—N3_1 | 84.90 (13) | O6_2—Ni2_2—N3_2 | 88.99 (11) |
O7_1—Ni1_1—O11_1 | 92.48 (13) | O9_2—Ni2_2—O11_2 | 152.77 (11) |
O6_1—Ni1_1—O11_1 | 87.75 (11) | O7_2—Ni2_2—O11_2 | 89.89 (12) |
O8_1—Ni1_1—O11_1 | 174.39 (10) | O6_2—Ni2_2—O11_2 | 88.39 (12) |
N3_1—Ni1_1—O11_1 | 95.76 (13) | N3_2—Ni2_2—O11_2 | 97.87 (13) |
O7_1—Ni1_1—O12_1 | 89.17 (11) | O9_2—Ni2_2—O12_2 | 91.87 (11) |
O6_1—Ni1_1—O12_1 | 87.95 (10) | O7_2—Ni2_2—O12_2 | 88.33 (10) |
O8_1—Ni1_1—O12_1 | 117.69 (10) | O6_2—Ni2_2—O12_2 | 89.75 (10) |
N3_1—Ni1_1—O12_1 | 157.23 (13) | N3_2—Ni2_2—O12_2 | 158.75 (13) |
O11_1—Ni1_1—O12_1 | 61.47 (10) | O11_2—Ni2_2—O12_2 | 60.90 (10) |
Ni1_1—O6_1—H6C_1 | 109 (2) | Ni2_2—O6_2—H6C_2 | 124 (3) |
Ni1_1—O6_1—H6D_1 | 130 (2) | Ni2_2—O6_2—H6D_2 | 120 (3) |
H6C_1—O6_1—H6D_1 | 104 (2) | H6C_2—O6_2—H6D_2 | 104 (2) |
Ni1_1—O7_1—H7C_1 | 122 (2) | Ni2_2—O7_2—H7C_2 | 124 (2) |
Ni1_1—O7_1—H7D_1 | 129 (2) | Ni2_2—O7_2—H7D_2 | 130 (2) |
H7C_1—O7_1—H7D_1 | 109 (3) | H7C_2—O7_2—H7D_2 | 105 (2) |
O9_1—N1_1—O10_1 | 119.7 (4) | O10_2—N1_2—O8_2 | 121.3 (4) |
O9_1—N1_1—O8_1 | 120.2 (4) | O10_2—N1_2—O9_2 | 119.0 (3) |
O10_1—N1_1—O8_1 | 120.0 (3) | O8_2—N1_2—O9_2 | 119.7 (3) |
N1_1—O8_1—Ni1_1 | 120.7 (2) | N1_2—O9_2—Ni2_2 | 125.9 (2) |
O13_1—N2_1—O12_1 | 121.9 (3) | O13_2—N2_2—O12_2 | 123.1 (3) |
O13_1—N2_1—O11_1 | 121.6 (4) | O13_2—N2_2—O11_2 | 122.2 (4) |
O12_1—N2_1—O11_1 | 116.5 (3) | O12_2—N2_2—O11_2 | 114.7 (3) |
N2_1—O11_1—Ni1_1 | 91.8 (2) | N2_2—O11_2—Ni2_2 | 92.3 (2) |
N2_1—O12_1—Ni1_1 | 90.3 (2) | N2_2—O12_2—Ni2_2 | 92.0 (2) |
C12_1—C11_1—H11A_1 | 109.5 | C12_2—C11_2—H11A_2 | 109.5 |
C12_1—C11_1—H11B_1 | 109.5 | C12_2—C11_2—H11B_2 | 109.5 |
H11A_1—C11_1—H11B_1 | 109.5 | H11A_2—C11_2—H11B_2 | 109.5 |
C12_1—C11_1—H11C_1 | 109.5 | C12_2—C11_2—H11C_2 | 109.5 |
H11A_1—C11_1—H11C_1 | 109.5 | H11A_2—C11_2—H11C_2 | 109.5 |
H11B_1—C11_1—H11C_1 | 109.5 | H11B_2—C11_2—H11C_2 | 109.5 |
N3_1—C12_1—C11_1 | 178.4 (4) | N3_2—C12_2—C11_2 | 177.4 (4) |
C12_1—N3_1—Ni1_1 | 164.2 (3) | C12_2—N3_2—Ni2_2 | 164.4 (3) |
C14_1—C13_1—H13A_1 | 109.5 | C14_2—C13_2—H13A_2 | 109.5 |
C14_1—C13_1—H13B_1 | 109.5 | C14_2—C13_2—H13B_2 | 109.5 |
H13A_1—C13_1—H13B_1 | 109.5 | H13A_2—C13_2—H13B_2 | 109.5 |
C14_1—C13_1—H13C_1 | 109.5 | C14_2—C13_2—H13C_2 | 109.5 |
H13A_1—C13_1—H13C_1 | 109.5 | H13A_2—C13_2—H13C_2 | 109.5 |
H13B_1—C13_1—H13C_1 | 109.5 | H13B_2—C13_2—H13C_2 | 109.5 |
N4_1—C14_1—C13_1 | 178.5 (5) | N4_2—C14_2—C13_2 | 179.0 (5) |
| | | |
O1_1—C1_1—C2_1—O2_1 | −61.0 (4) | O2_2—C3_2—C4_2—O3_2 | −74.4 (4) |
O2_1—C3_1—C4_1—O3_1 | 71.7 (4) | O3_2—C5_2—C6_2—O4_2 | −58.2 (4) |
O3_1—C5_1—C6_1—O4_1 | 58.8 (4) | O4_2—C7_2—C8_2—O5_2 | 77.2 (4) |
O4_1—C7_1—C8_1—O5_1 | −79.6 (4) | O5_2—C9_2—C10_2—O1_2 | −67.6 (4) |
O5_1—C9_1—C10_1—O1_1 | 68.6 (4) | C2_2—C1_2—O1_2—C10_2 | −168.2 (3) |
C9_1—C10_1—O1_1—C1_1 | −166.0 (3) | C9_2—C10_2—O1_2—C1_2 | 163.7 (3) |
C2_1—C1_1—O1_1—C10_1 | 166.9 (3) | C1_2—C2_2—O2_2—C3_2 | −175.8 (3) |
C4_1—C3_1—O2_1—C2_1 | −167.0 (3) | C4_2—C3_2—O2_2—C2_2 | 169.1 (3) |
C1_1—C2_1—O2_1—C3_1 | 176.2 (3) | C3_2—C4_2—O3_2—C5_2 | 170.8 (3) |
C6_1—C5_1—O3_1—C4_1 | 91.2 (4) | C6_2—C5_2—O3_2—C4_2 | −90.4 (4) |
C3_1—C4_1—O3_1—C5_1 | −171.4 (3) | C5_2—C6_2—O4_2—C7_2 | −178.8 (3) |
C5_1—C6_1—O4_1—C7_1 | −179.8 (3) | C8_2—C7_2—O4_2—C6_2 | −159.8 (3) |
C8_1—C7_1—O4_1—C6_1 | 160.6 (3) | C7_2—C8_2—O5_2—C9_2 | −167.4 (3) |
C10_1—C9_1—O5_1—C8_1 | −163.5 (3) | C10_2—C9_2—O5_2—C8_2 | 166.2 (3) |
C7_1—C8_1—O5_1—C9_1 | 166.7 (3) | O10_2—N1_2—O9_2—Ni2_2 | −173.4 (3) |
O9_1—N1_1—O8_1—Ni1_1 | 8.5 (4) | O8_2—N1_2—O9_2—Ni2_2 | 6.4 (5) |
O10_1—N1_1—O8_1—Ni1_1 | −169.1 (3) | O7_2—Ni2_2—O9_2—N1_2 | −116.8 (3) |
O7_1—Ni1_1—O8_1—N1_1 | −92.4 (3) | O6_2—Ni2_2—O9_2—N1_2 | 65.1 (3) |
O6_1—Ni1_1—O8_1—N1_1 | 84.2 (3) | N3_2—Ni2_2—O9_2—N1_2 | −24.5 (3) |
N3_1—Ni1_1—O8_1—N1_1 | 175.1 (3) | O11_2—Ni2_2—O9_2—N1_2 | 155.3 (3) |
O12_1—Ni1_1—O8_1—N1_1 | −1.7 (3) | O12_2—Ni2_2—O9_2—N1_2 | 154.9 (3) |
O13_1—N2_1—O11_1—Ni1_1 | 178.1 (4) | O13_2—N2_2—O11_2—Ni2_2 | 177.3 (4) |
O12_1—N2_1—O11_1—Ni1_1 | −1.4 (4) | O12_2—N2_2—O11_2—Ni2_2 | −2.6 (3) |
O7_1—Ni1_1—O11_1—N2_1 | 88.6 (2) | O9_2—Ni2_2—O11_2—N2_2 | 1.2 (4) |
O6_1—Ni1_1—O11_1—N2_1 | −88.0 (2) | O7_2—Ni2_2—O11_2—N2_2 | −86.5 (2) |
N3_1—Ni1_1—O11_1—N2_1 | −178.5 (2) | O6_2—Ni2_2—O11_2—N2_2 | 92.2 (2) |
O12_1—Ni1_1—O11_1—N2_1 | 0.9 (2) | N3_2—Ni2_2—O11_2—N2_2 | −179.0 (2) |
O13_1—N2_1—O12_1—Ni1_1 | −178.2 (4) | O12_2—Ni2_2—O11_2—N2_2 | 1.6 (2) |
O11_1—N2_1—O12_1—Ni1_1 | 1.4 (4) | O13_2—N2_2—O12_2—Ni2_2 | −177.3 (4) |
O7_1—Ni1_1—O12_1—N2_1 | −94.2 (2) | O11_2—N2_2—O12_2—Ni2_2 | 2.6 (3) |
O6_1—Ni1_1—O12_1—N2_1 | 87.7 (2) | O9_2—Ni2_2—O12_2—N2_2 | 178.1 (2) |
O8_1—Ni1_1—O12_1—N2_1 | 172.8 (2) | O7_2—Ni2_2—O12_2—N2_2 | 89.2 (2) |
N3_1—Ni1_1—O12_1—N2_1 | 0.8 (4) | O6_2—Ni2_2—O12_2—N2_2 | −89.9 (2) |
O11_1—Ni1_1—O12_1—N2_1 | −0.9 (2) | N3_2—Ni2_2—O12_2—N2_2 | −3.4 (4) |
O7_1—Ni1_1—N3_1—C12_1 | −173.1 (14) | O11_2—Ni2_2—O12_2—N2_2 | −1.6 (2) |
O6_1—Ni1_1—N3_1—C12_1 | 6.3 (14) | O9_2—Ni2_2—N3_2—C12_2 | 95.4 (13) |
O8_1—Ni1_1—N3_1—C12_1 | −80.2 (14) | O7_2—Ni2_2—N3_2—C12_2 | −174.8 (13) |
O11_1—Ni1_1—N3_1—C12_1 | 94.2 (14) | O6_2—Ni2_2—N3_2—C12_2 | 3.7 (13) |
O12_1—Ni1_1—N3_1—C12_1 | 92.6 (14) | O11_2—Ni2_2—N3_2—C12_2 | −84.5 (13) |
O1_2—C1_2—C2_2—O2_2 | 62.5 (4) | O12_2—Ni2_2—N3_2—C12_2 | −83.0 (14) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O6_1—H6C_1···O2_1 | 0.83 (2) | 1.89 (2) | 2.695 (4) | 164 (3) |
O6_1—H6D_1···O5_1 | 0.85 (2) | 1.94 (2) | 2.756 (4) | 161 (3) |
O7_1—H7C_1···O3_2i | 0.82 (2) | 2.04 (2) | 2.810 (3) | 157 (4) |
O7_1—H7D_1···O1_2i | 0.83 (2) | 2.01 (2) | 2.830 (3) | 173 (4) |
O6_2—H6C_2···O5_2 | 0.84 (2) | 1.91 (2) | 2.752 (4) | 178 (3) |
O6_2—H6D_2···O2_2 | 0.84 (2) | 1.88 (2) | 2.710 (4) | 170 (4) |
O7_2—H7C_2···O3_1 | 0.86 (2) | 1.93 (2) | 2.758 (4) | 161 (4) |
O7_2—H7D_2···O1_1 | 0.83 (2) | 2.02 (2) | 2.841 (3) | 172 (4) |
Symmetry code: (i) x, y, z−1. |
Crystal data top
C10H24O7Ni2+·2(NO3−) | F(000) = 2760 |
Mr = 439.02 | Dx = 1.682 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 12375 reflections |
a = 14.676 (1) Å | θ = 1.0–27.5° |
b = 13.961 (1) Å | µ = 1.19 mm−1 |
c = 25.552 (2) Å | T = 90 K |
β = 96.56 (1)° | Block, pale yellow |
V = 5201.1 (7) Å3 | 0.40 × 0.15 × 0.10 mm |
Z = 12 | |
Data collection top
Nonius KappaCCD diffractometer | 11918 independent reflections |
Radiation source: fine-focus sealed tube | 6757 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
Detector resolution: 18 pixels mm-1 | θmax = 27.5°, θmin = 1.4° |
ω scans at fixed χ = 55° | h = −19→19 |
Absorption correction: multi-scan Scalepack (Otwinowski & Minor, 2006) | k = −18→18 |
Tmin = 0.647, Tmax = 0.890 | l = −33→33 |
23212 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.102 | H 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 parameters | Δρmax = 0.42 e Å−3 |
18 restraints | Δρmin = −0.56 e Å−3 |
Special details top
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes. |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ni1_1 | 0.2459 (2) | 0.4976 (2) | 0.01306 (13) | 0.0149 (3) | 0.333 (6) |
Ni1'_1 | 0.27083 (19) | 0.50958 (13) | 0.00981 (6) | 0.0149 (3) | 0.667 (6) |
O1_1 | 0.38339 (9) | 0.53232 (10) | −0.03377 (5) | 0.0157 (3) | |
O2_1 | 0.34722 (9) | 0.60436 (10) | 0.05823 (5) | 0.0174 (4) | |
O3_1 | 0.20278 (9) | 0.51376 (10) | 0.08610 (5) | 0.0188 (4) | |
O4_1 | 0.11275 (10) | 0.43362 (10) | −0.00102 (5) | 0.0208 (4) | |
O5_1 | 0.23707 (9) | 0.43487 (10) | −0.06388 (5) | 0.0170 (3) | |
O6_1 | 0.32115 (12) | 0.38483 (11) | 0.03858 (6) | 0.0270 (4) | |
H6W1_1 | 0.3383 (16) | 0.3446 (13) | 0.0178 (6) | 0.040* | |
H6W2_1 | 0.3421 (15) | 0.3701 (16) | 0.0682 (4) | 0.040* | |
O7_1 | 0.20386 (11) | 0.62269 (11) | −0.02049 (6) | 0.0245 (4) | |
H7W1_1 | 0.1841 (15) | 0.6703 (12) | −0.0060 (7) | 0.037* | |
H7W2_1 | 0.1697 (13) | 0.6159 (15) | −0.0491 (5) | 0.037* | |
C1_1 | 0.43095 (14) | 0.61736 (15) | −0.01440 (8) | 0.0199 (5) | |
H1A_1 | 0.3960 | 0.6752 | −0.0269 | 0.024* | |
H1B_1 | 0.4924 | 0.6204 | −0.0268 | 0.024* | |
C2_1 | 0.43941 (14) | 0.61124 (16) | 0.04465 (8) | 0.0208 (5) | |
H2A_1 | 0.4755 | 0.5541 | 0.0572 | 0.025* | |
H2B_1 | 0.4701 | 0.6690 | 0.0607 | 0.025* | |
C3_1 | 0.34042 (14) | 0.59448 (16) | 0.11375 (8) | 0.0191 (5) | |
H3A_1 | 0.3701 | 0.6492 | 0.1336 | 0.023* | |
H3B_1 | 0.3700 | 0.5344 | 0.1275 | 0.023* | |
C4_1 | 0.23920 (14) | 0.59258 (15) | 0.11840 (8) | 0.0190 (5) | |
H4A_1 | 0.2280 | 0.5827 | 0.1555 | 0.023* | |
H4B_1 | 0.2101 | 0.6536 | 0.1057 | 0.023* | |
C5_1 | 0.10368 (14) | 0.50691 (16) | 0.08103 (8) | 0.0226 (6) | |
H5A_1 | 0.0755 | 0.5641 | 0.0629 | 0.027* | |
H5B_1 | 0.0818 | 0.5018 | 0.1162 | 0.027* | |
C6_1 | 0.07930 (15) | 0.41826 (17) | 0.04911 (8) | 0.0245 (6) | |
H6A_1 | 0.1087 | 0.3612 | 0.0668 | 0.029* | |
H6B_1 | 0.0120 | 0.4085 | 0.0445 | 0.029* | |
C7_1 | 0.11802 (15) | 0.34817 (15) | −0.03170 (8) | 0.0208 (5) | |
H7A_1 | 0.0562 | 0.3203 | −0.0408 | 0.025* | |
H7B_1 | 0.1575 | 0.3000 | −0.0118 | 0.025* | |
C8_1 | 0.15841 (14) | 0.37754 (16) | −0.08085 (8) | 0.0205 (5) | |
H8A_1 | 0.1764 | 0.3204 | −0.1002 | 0.025* | |
H8B_1 | 0.1133 | 0.4149 | −0.1044 | 0.025* | |
C9_1 | 0.30343 (14) | 0.44133 (15) | −0.10078 (8) | 0.0174 (5) | |
H9A_1 | 0.2726 | 0.4406 | −0.1373 | 0.021* | |
H9B_1 | 0.3466 | 0.3867 | −0.0963 | 0.021* | |
C10_1 | 0.35397 (14) | 0.53437 (15) | −0.08964 (8) | 0.0173 (5) | |
H10A_1 | 0.4073 | 0.5387 | −0.1100 | 0.021* | |
H10B_1 | 0.3130 | 0.5897 | −0.0988 | 0.021* | |
Ni2_2 | 0.26091 (16) | 0.5013 (2) | 0.32716 (13) | 0.0148 (3) | 0.435 (4) |
Ni2'_2 | 0.23445 (17) | 0.49127 (17) | 0.32948 (9) | 0.0148 (3) | 0.565 (4) |
O1_2 | 0.11725 (9) | 0.47590 (10) | 0.36888 (5) | 0.0177 (4) | |
O2_2 | 0.15809 (9) | 0.39734 (10) | 0.27946 (5) | 0.0185 (4) | |
O3_2 | 0.30631 (10) | 0.48202 (10) | 0.25346 (5) | 0.0190 (4) | |
O4_2 | 0.39393 (10) | 0.56151 (10) | 0.34150 (5) | 0.0187 (4) | |
O5_2 | 0.26889 (10) | 0.56265 (10) | 0.40375 (5) | 0.0186 (4) | |
O6_2 | 0.19608 (11) | 0.61931 (11) | 0.29929 (6) | 0.0253 (4) | |
H6W1_2 | 0.1779 (14) | 0.6592 (14) | 0.3198 (6) | 0.038* | |
H6W2_2 | 0.1597 (13) | 0.6207 (16) | 0.2720 (5) | 0.038* | |
O7_2 | 0.29764 (11) | 0.37620 (11) | 0.36100 (6) | 0.0241 (4) | |
H7W1_2 | 0.3375 (12) | 0.3800 (15) | 0.3870 (6) | 0.036* | |
H7W2_2 | 0.3096 (14) | 0.3265 (11) | 0.3453 (7) | 0.036* | |
C1_2 | 0.06853 (15) | 0.39101 (16) | 0.34966 (8) | 0.0217 (5) | |
H1A_2 | 0.0058 | 0.3907 | 0.3604 | 0.026* | |
H1B_2 | 0.1011 | 0.3328 | 0.3639 | 0.026* | |
C2_2 | 0.06484 (14) | 0.39381 (16) | 0.29070 (8) | 0.0221 (6) | |
H2A_2 | 0.0339 | 0.3359 | 0.2749 | 0.026* | |
H2B_2 | 0.0309 | 0.4511 | 0.2764 | 0.026* | |
C3_2 | 0.16862 (14) | 0.40189 (16) | 0.22431 (8) | 0.0195 (5) | |
H3A_2 | 0.1397 | 0.4606 | 0.2083 | 0.023* | |
H3B_2 | 0.1400 | 0.3455 | 0.2056 | 0.023* | |
C4_2 | 0.27017 (14) | 0.40298 (15) | 0.22141 (8) | 0.0200 (5) | |
H4A_2 | 0.2982 | 0.3420 | 0.2349 | 0.024* | |
H4B_2 | 0.2832 | 0.4116 | 0.1845 | 0.024* | |
C5_2 | 0.40499 (14) | 0.48708 (16) | 0.25993 (8) | 0.0213 (5) | |
H5A_2 | 0.4286 | 0.4915 | 0.2252 | 0.026* | |
H5B_2 | 0.4315 | 0.4294 | 0.2784 | 0.026* | |
C6_2 | 0.42962 (15) | 0.57516 (16) | 0.29189 (8) | 0.0222 (6) | |
H6A_2 | 0.4970 | 0.5835 | 0.2974 | 0.027* | |
H6B_2 | 0.4020 | 0.6326 | 0.2737 | 0.027* | |
C7_2 | 0.39129 (15) | 0.64686 (15) | 0.37208 (8) | 0.0208 (5) | |
H7A_2 | 0.3542 | 0.6967 | 0.3520 | 0.025* | |
H7B_2 | 0.4540 | 0.6720 | 0.3817 | 0.025* | |
C8_2 | 0.34821 (14) | 0.61927 (15) | 0.42084 (8) | 0.0211 (5) | |
H8A_2 | 0.3921 | 0.5819 | 0.4451 | 0.025* | |
H8B_2 | 0.3304 | 0.6773 | 0.4395 | 0.025* | |
C9_2 | 0.19747 (14) | 0.56401 (15) | 0.43745 (8) | 0.0187 (5) | |
H9A_2 | 0.1590 | 0.6220 | 0.4307 | 0.022* | |
H9B_2 | 0.2238 | 0.5640 | 0.4749 | 0.022* | |
C10_2 | 0.14127 (15) | 0.47525 (16) | 0.42501 (8) | 0.0208 (5) | |
H10A_2 | 0.1773 | 0.4173 | 0.4360 | 0.025* | |
H10B_2 | 0.0854 | 0.4763 | 0.4434 | 0.025* | |
Ni3_3 | 0.25743 (18) | 0.5070 (2) | 0.65864 (14) | 0.0141 (3) | 0.402 (5) |
Ni3'_3 | 0.23321 (17) | 0.49364 (16) | 0.66117 (8) | 0.0141 (3) | 0.598 (5) |
O1_3 | 0.12139 (9) | 0.46825 (10) | 0.70640 (5) | 0.0179 (4) | |
O2_3 | 0.16238 (9) | 0.39354 (10) | 0.61585 (5) | 0.0185 (4) | |
O3_3 | 0.29852 (9) | 0.49368 (10) | 0.58486 (5) | 0.0186 (4) | |
O4_3 | 0.38489 (10) | 0.58417 (11) | 0.66884 (6) | 0.0226 (4) | |
O5_3 | 0.26557 (10) | 0.56999 (10) | 0.73541 (5) | 0.0188 (4) | |
O6_3 | 0.17382 (12) | 0.61187 (11) | 0.63074 (6) | 0.0238 (4) | |
H6W1_3 | 0.1580 (16) | 0.6555 (12) | 0.6499 (6) | 0.036* | |
H6W2_3 | 0.1673 (16) | 0.6326 (14) | 0.6002 (4) | 0.036* | |
O7_3 | 0.31191 (12) | 0.38859 (12) | 0.69242 (6) | 0.0291 (4) | |
H7W1_3 | 0.3292 (15) | 0.3398 (12) | 0.6780 (8) | 0.044* | |
H7W2_3 | 0.3450 (14) | 0.3963 (16) | 0.7205 (6) | 0.044* | |
C1_3 | 0.07827 (16) | 0.37967 (16) | 0.68855 (8) | 0.0247 (6) | |
H1A_3 | 0.0170 | 0.3741 | 0.7009 | 0.030* | |
H1B_3 | 0.1161 | 0.3244 | 0.7022 | 0.030* | |
C2_3 | 0.06993 (15) | 0.38216 (17) | 0.62929 (8) | 0.0250 (6) | |
H2A_3 | 0.0426 | 0.3219 | 0.6143 | 0.030* | |
H2B_3 | 0.0309 | 0.4365 | 0.6155 | 0.030* | |
C3_3 | 0.16820 (14) | 0.39961 (16) | 0.56014 (8) | 0.0211 (5) | |
H3A_3 | 0.1335 | 0.4556 | 0.5447 | 0.025* | |
H3B_3 | 0.1434 | 0.3409 | 0.5420 | 0.025* | |
C4_3 | 0.26893 (14) | 0.41025 (15) | 0.55509 (8) | 0.0194 (5) | |
H4A_3 | 0.3031 | 0.3531 | 0.5693 | 0.023* | |
H4B_3 | 0.2790 | 0.4183 | 0.5177 | 0.023* | |
C5_3 | 0.39475 (14) | 0.51429 (17) | 0.58600 (9) | 0.0246 (6) | |
H5A_3 | 0.4112 | 0.5234 | 0.5498 | 0.030* | |
H5B_3 | 0.4319 | 0.4610 | 0.6028 | 0.030* | |
C6_3 | 0.41152 (16) | 0.60431 (17) | 0.61742 (8) | 0.0275 (6) | |
H6A_3 | 0.4771 | 0.6224 | 0.6201 | 0.033* | |
H6B_3 | 0.3745 | 0.6576 | 0.6006 | 0.033* | |
C7_3 | 0.37453 (15) | 0.66782 (15) | 0.70005 (8) | 0.0215 (5) | |
H7A_3 | 0.3298 | 0.7125 | 0.6812 | 0.026* | |
H7B_3 | 0.4340 | 0.7013 | 0.7078 | 0.026* | |
C8_3 | 0.34055 (15) | 0.63363 (16) | 0.75018 (8) | 0.0226 (6) | |
H8A_3 | 0.3901 | 0.5998 | 0.7724 | 0.027* | |
H8B_3 | 0.3200 | 0.6886 | 0.7703 | 0.027* | |
C9_3 | 0.19840 (14) | 0.56443 (15) | 0.77174 (8) | 0.0170 (5) | |
H9A_3 | 0.1543 | 0.6181 | 0.7659 | 0.020* | |
H9B_3 | 0.2283 | 0.5678 | 0.8084 | 0.020* | |
C10_3 | 0.14982 (15) | 0.47033 (16) | 0.76211 (8) | 0.0193 (5) | |
H10A_3 | 0.1916 | 0.4163 | 0.7726 | 0.023* | |
H10B_3 | 0.0961 | 0.4664 | 0.7822 | 0.023* | |
N1_4 | 0.10425 (12) | 0.68157 (13) | −0.14161 (7) | 0.0174 (4) | |
O8_4 | 0.10097 (10) | 0.60490 (10) | −0.11575 (6) | 0.0216 (4) | |
O9_4 | 0.17420 (11) | 0.73466 (11) | −0.13243 (6) | 0.0260 (4) | |
O10_4 | 0.04194 (10) | 0.70379 (11) | −0.17607 (6) | 0.0289 (4) | |
N2_5 | 0.07968 (12) | 0.68843 (13) | 0.18278 (7) | 0.0180 (4) | |
O8_5 | 0.06941 (10) | 0.61548 (11) | 0.21104 (6) | 0.0246 (4) | |
O9_5 | 0.14205 (10) | 0.74729 (10) | 0.19845 (5) | 0.0231 (4) | |
O10_5 | 0.03073 (10) | 0.70053 (11) | 0.14086 (6) | 0.0276 (4) | |
N3_6 | 0.08160 (13) | 0.68713 (13) | 0.51131 (7) | 0.0186 (4) | |
O8_6 | 0.04813 (11) | 0.61068 (11) | 0.52497 (7) | 0.0364 (5) | |
O9_6 | 0.15743 (10) | 0.71575 (11) | 0.53537 (6) | 0.0249 (4) | |
O10_6 | 0.04359 (10) | 0.73542 (11) | 0.47444 (6) | 0.0263 (4) | |
N4_7 | 0.42588 (12) | 0.30854 (13) | 0.15752 (7) | 0.0177 (4) | |
O8_7 | 0.45472 (12) | 0.38145 (11) | 0.13683 (7) | 0.0378 (5) | |
O9_7 | 0.35490 (10) | 0.26772 (12) | 0.13532 (6) | 0.0291 (4) | |
O10_7 | 0.46409 (10) | 0.27645 (11) | 0.19949 (6) | 0.0271 (4) | |
N5_8 | 0.40805 (12) | 0.31679 (13) | 0.48085 (7) | 0.0164 (4) | |
O8_8 | 0.41209 (10) | 0.39040 (10) | 0.45265 (6) | 0.0221 (4) | |
O9_8 | 0.34480 (10) | 0.25679 (11) | 0.46855 (6) | 0.0240 (4) | |
O10_8 | 0.46365 (10) | 0.30401 (11) | 0.52035 (6) | 0.0280 (4) | |
N6_9 | 0.39680 (12) | 0.32119 (13) | 0.81302 (7) | 0.0178 (4) | |
O8_9 | 0.41368 (10) | 0.39747 (11) | 0.78925 (6) | 0.0251 (4) | |
O9_9 | 0.31868 (10) | 0.28326 (10) | 0.80277 (5) | 0.0215 (4) | |
O10_9 | 0.45461 (10) | 0.28541 (11) | 0.84637 (6) | 0.0253 (4) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1_1 | 0.0160 (8) | 0.0142 (4) | 0.0144 (2) | 0.0024 (5) | 0.0013 (4) | 0.0001 (2) |
Ni1'_1 | 0.0160 (8) | 0.0142 (4) | 0.0144 (2) | 0.0024 (5) | 0.0013 (4) | 0.0001 (2) |
O1_1 | 0.0170 (8) | 0.0166 (9) | 0.0135 (7) | −0.0025 (7) | 0.0011 (6) | 0.0002 (7) |
O2_1 | 0.0171 (8) | 0.0199 (9) | 0.0152 (8) | 0.0024 (7) | 0.0025 (7) | −0.0007 (7) |
O3_1 | 0.0170 (8) | 0.0198 (9) | 0.0195 (8) | −0.0010 (7) | 0.0014 (7) | −0.0046 (7) |
O4_1 | 0.0243 (9) | 0.0214 (9) | 0.0176 (8) | −0.0044 (7) | 0.0059 (7) | −0.0025 (7) |
O5_1 | 0.0158 (8) | 0.0205 (9) | 0.0149 (8) | −0.0034 (7) | 0.0030 (7) | −0.0029 (7) |
O6_1 | 0.0460 (11) | 0.0199 (10) | 0.0140 (8) | 0.0159 (8) | −0.0015 (8) | −0.0013 (7) |
O7_1 | 0.0308 (10) | 0.0216 (10) | 0.0189 (9) | 0.0127 (8) | −0.0063 (7) | −0.0038 (7) |
C1_1 | 0.0187 (13) | 0.0172 (13) | 0.0245 (13) | −0.0038 (11) | 0.0051 (10) | −0.0011 (10) |
C2_1 | 0.0162 (13) | 0.0218 (14) | 0.0249 (13) | −0.0019 (11) | 0.0044 (10) | −0.0055 (11) |
C3_1 | 0.0244 (13) | 0.0186 (13) | 0.0141 (11) | −0.0017 (11) | 0.0012 (10) | −0.0047 (10) |
C4_1 | 0.0245 (13) | 0.0167 (13) | 0.0162 (11) | 0.0027 (10) | 0.0039 (10) | −0.0037 (10) |
C5_1 | 0.0179 (13) | 0.0308 (15) | 0.0201 (12) | 0.0004 (11) | 0.0058 (10) | −0.0022 (11) |
C6_1 | 0.0230 (13) | 0.0320 (15) | 0.0199 (12) | −0.0077 (11) | 0.0086 (11) | −0.0011 (11) |
C7_1 | 0.0214 (13) | 0.0153 (13) | 0.0254 (13) | −0.0058 (10) | 0.0010 (11) | −0.0038 (11) |
C8_1 | 0.0223 (13) | 0.0191 (13) | 0.0193 (12) | −0.0043 (11) | −0.0013 (10) | −0.0050 (10) |
C9_1 | 0.0203 (13) | 0.0185 (13) | 0.0135 (11) | 0.0009 (10) | 0.0030 (10) | −0.0020 (10) |
C10_1 | 0.0186 (13) | 0.0200 (13) | 0.0138 (11) | 0.0009 (11) | 0.0038 (10) | 0.0028 (10) |
Ni2_2 | 0.0152 (9) | 0.0129 (5) | 0.0163 (3) | 0.0009 (6) | 0.0015 (6) | 0.0010 (3) |
Ni2'_2 | 0.0152 (9) | 0.0129 (5) | 0.0163 (3) | 0.0009 (6) | 0.0015 (6) | 0.0010 (3) |
O1_2 | 0.0194 (9) | 0.0190 (9) | 0.0146 (8) | −0.0026 (7) | 0.0006 (7) | −0.0008 (7) |
O2_2 | 0.0182 (9) | 0.0214 (9) | 0.0163 (8) | −0.0005 (7) | 0.0031 (7) | −0.0011 (7) |
O3_2 | 0.0172 (9) | 0.0186 (9) | 0.0209 (8) | −0.0006 (7) | 0.0007 (7) | −0.0052 (7) |
O4_2 | 0.0219 (9) | 0.0181 (9) | 0.0166 (8) | −0.0027 (7) | 0.0038 (7) | −0.0013 (7) |
O5_2 | 0.0175 (8) | 0.0203 (9) | 0.0185 (8) | −0.0044 (7) | 0.0045 (7) | −0.0052 (7) |
O6_2 | 0.0395 (11) | 0.0194 (10) | 0.0160 (9) | 0.0116 (8) | −0.0011 (8) | −0.0016 (7) |
O7_2 | 0.0359 (11) | 0.0150 (9) | 0.0189 (9) | 0.0111 (8) | −0.0074 (8) | −0.0037 (7) |
C1_2 | 0.0202 (13) | 0.0202 (14) | 0.0247 (13) | −0.0040 (11) | 0.0024 (10) | 0.0000 (11) |
C2_2 | 0.0193 (13) | 0.0262 (14) | 0.0208 (12) | −0.0042 (11) | 0.0029 (10) | −0.0009 (11) |
C3_2 | 0.0265 (13) | 0.0181 (13) | 0.0135 (11) | −0.0030 (11) | −0.0001 (10) | −0.0045 (10) |
C4_2 | 0.0259 (14) | 0.0180 (13) | 0.0158 (11) | 0.0034 (11) | 0.0013 (10) | −0.0019 (10) |
C5_2 | 0.0177 (13) | 0.0261 (14) | 0.0205 (12) | −0.0013 (11) | 0.0038 (10) | −0.0022 (11) |
C6_2 | 0.0214 (13) | 0.0266 (15) | 0.0198 (12) | −0.0026 (11) | 0.0069 (10) | 0.0014 (11) |
C7_2 | 0.0227 (13) | 0.0184 (13) | 0.0213 (12) | −0.0047 (11) | 0.0022 (10) | −0.0035 (10) |
C8_2 | 0.0203 (13) | 0.0191 (13) | 0.0232 (13) | −0.0059 (11) | 0.0001 (10) | −0.0032 (11) |
C9_2 | 0.0206 (13) | 0.0222 (14) | 0.0143 (11) | 0.0025 (11) | 0.0065 (10) | 0.0005 (10) |
C10_2 | 0.0234 (13) | 0.0261 (14) | 0.0127 (11) | −0.0030 (11) | 0.0017 (10) | 0.0021 (10) |
Ni3_3 | 0.0146 (8) | 0.0126 (6) | 0.0152 (3) | 0.0000 (5) | 0.0018 (6) | 0.0006 (3) |
Ni3'_3 | 0.0146 (8) | 0.0126 (6) | 0.0152 (3) | 0.0000 (5) | 0.0018 (6) | 0.0006 (3) |
O1_3 | 0.0198 (9) | 0.0168 (9) | 0.0164 (8) | −0.0037 (7) | −0.0008 (7) | −0.0017 (7) |
O2_3 | 0.0175 (8) | 0.0198 (9) | 0.0189 (8) | −0.0009 (7) | 0.0047 (7) | −0.0002 (7) |
O3_3 | 0.0161 (8) | 0.0223 (9) | 0.0172 (8) | −0.0014 (7) | 0.0003 (7) | −0.0033 (7) |
O4_3 | 0.0260 (9) | 0.0247 (10) | 0.0180 (8) | −0.0027 (8) | 0.0060 (7) | −0.0030 (7) |
O5_3 | 0.0182 (8) | 0.0224 (9) | 0.0160 (8) | −0.0050 (7) | 0.0029 (7) | −0.0041 (7) |
O6_3 | 0.0394 (11) | 0.0191 (10) | 0.0129 (8) | 0.0127 (8) | 0.0026 (8) | 0.0000 (7) |
O7_3 | 0.0399 (11) | 0.0255 (11) | 0.0201 (9) | 0.0160 (9) | −0.0039 (8) | −0.0008 (8) |
C1_3 | 0.0248 (14) | 0.0220 (14) | 0.0283 (14) | −0.0057 (11) | 0.0080 (11) | −0.0066 (11) |
C2_3 | 0.0227 (14) | 0.0263 (15) | 0.0269 (13) | −0.0073 (11) | 0.0061 (11) | −0.0093 (11) |
C3_3 | 0.0264 (14) | 0.0217 (14) | 0.0147 (12) | −0.0006 (11) | 0.0010 (10) | −0.0060 (10) |
C4_3 | 0.0267 (14) | 0.0179 (13) | 0.0134 (11) | 0.0059 (11) | 0.0019 (10) | −0.0025 (10) |
C5_3 | 0.0189 (13) | 0.0337 (16) | 0.0217 (12) | −0.0042 (11) | 0.0037 (10) | −0.0025 (11) |
C6_3 | 0.0245 (14) | 0.0381 (16) | 0.0212 (13) | −0.0104 (12) | 0.0087 (11) | −0.0016 (12) |
C7_3 | 0.0241 (13) | 0.0194 (13) | 0.0215 (12) | −0.0064 (11) | 0.0049 (10) | −0.0050 (10) |
C8_3 | 0.0225 (13) | 0.0245 (14) | 0.0206 (12) | −0.0066 (11) | 0.0009 (10) | −0.0051 (11) |
C9_3 | 0.0208 (13) | 0.0191 (13) | 0.0116 (11) | 0.0026 (10) | 0.0038 (10) | −0.0013 (10) |
C10_3 | 0.0237 (14) | 0.0204 (13) | 0.0137 (11) | 0.0018 (11) | 0.0024 (10) | 0.0037 (10) |
N1_4 | 0.0218 (11) | 0.0163 (11) | 0.0144 (10) | 0.0023 (9) | 0.0035 (9) | −0.0025 (9) |
O8_4 | 0.0290 (9) | 0.0154 (9) | 0.0200 (8) | −0.0032 (7) | 0.0014 (7) | 0.0055 (7) |
O9_4 | 0.0332 (10) | 0.0223 (10) | 0.0214 (9) | −0.0110 (8) | −0.0009 (7) | 0.0018 (7) |
O10_4 | 0.0274 (9) | 0.0328 (11) | 0.0242 (9) | 0.0117 (8) | −0.0065 (8) | 0.0030 (8) |
N2_5 | 0.0201 (11) | 0.0150 (11) | 0.0194 (10) | 0.0031 (9) | 0.0040 (9) | −0.0021 (9) |
O8_5 | 0.0305 (10) | 0.0173 (9) | 0.0265 (9) | −0.0033 (8) | 0.0059 (8) | 0.0035 (7) |
O9_5 | 0.0302 (10) | 0.0176 (9) | 0.0205 (9) | −0.0103 (8) | −0.0015 (7) | −0.0014 (7) |
O10_5 | 0.0292 (9) | 0.0253 (10) | 0.0246 (9) | 0.0042 (8) | −0.0129 (8) | −0.0023 (8) |
N3_6 | 0.0232 (11) | 0.0156 (11) | 0.0180 (10) | −0.0015 (9) | 0.0072 (9) | −0.0023 (9) |
O8_6 | 0.0387 (11) | 0.0215 (10) | 0.0508 (12) | −0.0070 (9) | 0.0129 (9) | 0.0107 (9) |
O9_6 | 0.0259 (9) | 0.0271 (10) | 0.0200 (8) | −0.0044 (8) | −0.0049 (7) | −0.0030 (7) |
O10_6 | 0.0264 (9) | 0.0283 (10) | 0.0230 (9) | 0.0057 (8) | −0.0030 (7) | 0.0049 (8) |
N4_7 | 0.0191 (11) | 0.0163 (11) | 0.0182 (10) | 0.0026 (9) | 0.0044 (9) | −0.0005 (9) |
O8_7 | 0.0525 (12) | 0.0173 (10) | 0.0490 (12) | −0.0048 (9) | 0.0287 (10) | 0.0076 (9) |
O9_7 | 0.0271 (10) | 0.0365 (11) | 0.0218 (9) | −0.0081 (8) | −0.0050 (8) | −0.0053 (8) |
O10_7 | 0.0275 (9) | 0.0307 (10) | 0.0208 (9) | 0.0072 (8) | −0.0073 (7) | 0.0009 (8) |
N5_8 | 0.0178 (11) | 0.0155 (11) | 0.0165 (10) | 0.0000 (9) | 0.0038 (9) | −0.0031 (8) |
O8_8 | 0.0306 (10) | 0.0170 (9) | 0.0188 (8) | −0.0055 (7) | 0.0030 (7) | 0.0040 (7) |
O9_8 | 0.0322 (10) | 0.0183 (9) | 0.0203 (8) | −0.0100 (8) | −0.0023 (7) | 0.0016 (7) |
O10_8 | 0.0275 (9) | 0.0260 (10) | 0.0271 (9) | 0.0038 (8) | −0.0117 (8) | 0.0029 (8) |
N6_9 | 0.0211 (11) | 0.0167 (11) | 0.0160 (10) | 0.0031 (9) | 0.0040 (9) | −0.0017 (9) |
O8_9 | 0.0318 (10) | 0.0193 (9) | 0.0242 (9) | −0.0080 (8) | 0.0027 (8) | 0.0031 (7) |
O9_9 | 0.0211 (9) | 0.0188 (9) | 0.0231 (9) | −0.0055 (7) | −0.0031 (7) | 0.0019 (7) |
O10_9 | 0.0218 (9) | 0.0300 (10) | 0.0223 (9) | 0.0058 (8) | −0.0054 (7) | 0.0011 (8) |
Geometric parameters (Å, º) top
Ni1_1—O6_1 | 1.989 (4) | C4_2—H4A_2 | 0.9900 |
Ni1_1—O7_1 | 2.011 (4) | C4_2—H4B_2 | 0.9900 |
Ni1_1—O3_1 | 2.050 (3) | C5_2—C6_2 | 1.497 (3) |
Ni1_1—O4_1 | 2.141 (3) | C5_2—H5A_2 | 0.9900 |
Ni1_1—O5_1 | 2.142 (4) | C5_2—H5B_2 | 0.9900 |
Ni1_1—O2_1 | 2.318 (3) | C6_2—H6A_2 | 0.9900 |
Ni1_1—O1_1 | 2.508 (3) | C6_2—H6B_2 | 0.9900 |
Ni1'_1—O7_1 | 1.971 (2) | C7_2—C8_2 | 1.510 (3) |
Ni1'_1—O6_1 | 1.999 (2) | C7_2—H7A_2 | 0.9900 |
Ni1'_1—O2_1 | 2.055 (3) | C7_2—H7B_2 | 0.9900 |
Ni1'_1—O1_1 | 2.119 (3) | C8_2—H8A_2 | 0.9900 |
Ni1'_1—O5_1 | 2.160 (2) | C8_2—H8B_2 | 0.9900 |
Ni1'_1—O3_1 | 2.290 (3) | C9_2—C10_2 | 1.502 (3) |
Ni1'_1—O4_1 | 2.537 (3) | C9_2—H9A_2 | 0.9900 |
O1_1—C1_1 | 1.436 (2) | C9_2—H9B_2 | 0.9900 |
O1_1—C10_1 | 1.444 (2) | C10_2—H10A_2 | 0.9900 |
O2_1—C2_1 | 1.438 (2) | C10_2—H10B_2 | 0.9900 |
O2_1—C3_1 | 1.440 (2) | Ni3_3—O7_3 | 1.989 (4) |
O3_1—C4_1 | 1.441 (2) | Ni3_3—O6_3 | 1.990 (4) |
O3_1—C5_1 | 1.449 (2) | Ni3_3—O3_3 | 2.052 (4) |
O4_1—C7_1 | 1.434 (2) | Ni3_3—O5_3 | 2.141 (4) |
O4_1—C6_1 | 1.439 (2) | Ni3_3—O4_3 | 2.149 (3) |
O5_1—C8_1 | 1.431 (2) | Ni3_3—O2_3 | 2.302 (3) |
O5_1—C9_1 | 1.434 (2) | Ni3_3—O1_3 | 2.515 (3) |
O6_1—H6W1_1 | 0.831 (9) | Ni3'_3—O7_3 | 1.978 (3) |
O6_1—H6W2_1 | 0.812 (9) | Ni3'_3—O6_3 | 1.983 (3) |
O7_1—H7W1_1 | 0.830 (9) | Ni3'_3—O2_3 | 2.025 (3) |
O7_1—H7W2_1 | 0.844 (9) | Ni3'_3—O1_3 | 2.142 (3) |
C1_1—C2_1 | 1.502 (3) | Ni3'_3—O5_3 | 2.180 (3) |
C1_1—H1A_1 | 0.9900 | Ni3'_3—O3_3 | 2.269 (3) |
C1_1—H1B_1 | 0.9900 | Ni3'_3—O4_3 | 2.548 (3) |
C2_1—H2A_1 | 0.9900 | O1_3—C10_3 | 1.437 (2) |
C2_1—H2B_1 | 0.9900 | O1_3—C1_3 | 1.439 (2) |
C3_1—C4_1 | 1.504 (3) | O2_3—C3_3 | 1.438 (2) |
C3_1—H3A_1 | 0.9900 | O2_3—C2_3 | 1.446 (2) |
C3_1—H3B_1 | 0.9900 | O3_3—C4_3 | 1.431 (2) |
C4_1—H4A_1 | 0.9900 | O3_3—C5_3 | 1.438 (2) |
C4_1—H4B_1 | 0.9900 | O4_3—C7_3 | 1.432 (2) |
C5_1—C6_1 | 1.503 (3) | O4_3—C6_3 | 1.441 (2) |
C5_1—H5A_1 | 0.9900 | O5_3—C8_3 | 1.431 (2) |
C5_1—H5B_1 | 0.9900 | O5_3—C9_3 | 1.431 (2) |
C6_1—H6A_1 | 0.9900 | O6_3—H6W1_3 | 0.831 (9) |
C6_1—H6B_1 | 0.9900 | O6_3—H6W2_3 | 0.828 (9) |
C7_1—C8_1 | 1.506 (3) | O7_3—H7W1_3 | 0.828 (9) |
C7_1—H7A_1 | 0.9900 | O7_3—H7W2_3 | 0.827 (9) |
C7_1—H7B_1 | 0.9900 | C1_3—C2_3 | 1.506 (3) |
C8_1—H8A_1 | 0.9900 | C1_3—H1A_3 | 0.9900 |
C8_1—H8B_1 | 0.9900 | C1_3—H1B_3 | 0.9900 |
C9_1—C10_1 | 1.507 (3) | C2_3—H2A_3 | 0.9900 |
C9_1—H9A_1 | 0.9900 | C2_3—H2B_3 | 0.9900 |
C9_1—H9B_1 | 0.9900 | C3_3—C4_3 | 1.506 (3) |
C10_1—H10A_1 | 0.9900 | C3_3—H3A_3 | 0.9900 |
C10_1—H10B_1 | 0.9900 | C3_3—H3B_3 | 0.9900 |
Ni2_2—O6_2 | 1.993 (3) | C4_3—H4A_3 | 0.9900 |
Ni2_2—O7_2 | 1.995 (3) | C4_3—H4B_3 | 0.9900 |
Ni2_2—O3_2 | 2.085 (4) | C5_3—C6_3 | 1.497 (3) |
Ni2_2—O4_2 | 2.119 (3) | C5_3—H5A_3 | 0.9900 |
Ni2_2—O5_2 | 2.127 (4) | C5_3—H5B_3 | 0.9900 |
Ni2_2—O2_2 | 2.334 (3) | C6_3—H6A_3 | 0.9900 |
Ni2_2—O1_2 | 2.494 (3) | C6_3—H6B_3 | 0.9900 |
Ni2'_2—O7_2 | 1.980 (3) | C7_3—C8_3 | 1.505 (3) |
Ni2'_2—O6_2 | 2.002 (3) | C7_3—H7A_3 | 0.9900 |
Ni2'_2—O2_2 | 2.069 (3) | C7_3—H7B_3 | 0.9900 |
Ni2'_2—O1_2 | 2.101 (3) | C8_3—H8A_3 | 0.9900 |
Ni2'_2—O5_2 | 2.152 (3) | C8_3—H8B_3 | 0.9900 |
Ni2'_2—O3_2 | 2.317 (3) | C9_3—C10_3 | 1.502 (3) |
Ni2'_2—O4_2 | 2.524 (3) | C9_3—H9A_3 | 0.9900 |
O1_2—C10_2 | 1.437 (2) | C9_3—H9B_3 | 0.9900 |
O1_2—C1_2 | 1.441 (2) | C10_3—H10A_3 | 0.9900 |
O2_2—C2_2 | 1.431 (2) | C10_3—H10B_3 | 0.9900 |
O2_2—C3_2 | 1.436 (2) | N1_4—O10_4 | 1.235 (2) |
O3_2—C4_2 | 1.439 (2) | N1_4—O8_4 | 1.262 (2) |
O3_2—C5_2 | 1.440 (2) | N1_4—O9_4 | 1.266 (2) |
O4_2—C7_2 | 1.428 (2) | N2_5—O10_5 | 1.231 (2) |
O4_2—C6_2 | 1.438 (2) | N2_5—O9_5 | 1.261 (2) |
O5_2—C9_2 | 1.431 (2) | N2_5—O8_5 | 1.267 (2) |
O5_2—C8_2 | 1.433 (2) | N3_6—O10_6 | 1.238 (2) |
O6_2—H6W1_2 | 0.829 (9) | N3_6—O8_6 | 1.242 (2) |
O6_2—H6W2_2 | 0.828 (9) | N3_6—O9_6 | 1.273 (2) |
O7_2—H7W1_2 | 0.835 (9) | N4_7—O10_7 | 1.236 (2) |
O7_2—H7W2_2 | 0.831 (9) | N4_7—O8_7 | 1.243 (2) |
C1_2—C2_2 | 1.502 (3) | N4_7—O9_7 | 1.264 (2) |
C1_2—H1A_2 | 0.9900 | N5_8—O10_8 | 1.236 (2) |
C1_2—H1B_2 | 0.9900 | N5_8—O8_8 | 1.260 (2) |
C2_2—H2A_2 | 0.9900 | N5_8—O9_8 | 1.263 (2) |
C2_2—H2B_2 | 0.9900 | N6_9—O10_9 | 1.237 (2) |
C3_2—C4_2 | 1.501 (3) | N6_9—O9_9 | 1.263 (2) |
C3_2—H3A_2 | 0.9900 | N6_9—O8_9 | 1.264 (2) |
C3_2—H3B_2 | 0.9900 | | |
| | | |
O6_1—Ni1_1—O7_1 | 163.42 (18) | O1_2—C1_2—H1A_2 | 110.5 |
O6_1—Ni1_1—O3_1 | 90.37 (14) | C2_2—C1_2—H1A_2 | 110.5 |
O7_1—Ni1_1—O3_1 | 100.42 (16) | O1_2—C1_2—H1B_2 | 110.5 |
O6_1—Ni1_1—O4_1 | 100.79 (16) | C2_2—C1_2—H1B_2 | 110.5 |
O7_1—Ni1_1—O4_1 | 93.50 (14) | H1A_2—C1_2—H1B_2 | 108.7 |
O3_1—Ni1_1—O4_1 | 80.13 (12) | O2_2—C2_2—C1_2 | 106.06 (17) |
O6_1—Ni1_1—O5_1 | 87.17 (14) | O2_2—C2_2—H2A_2 | 110.5 |
O7_1—Ni1_1—O5_1 | 88.86 (14) | C1_2—C2_2—H2A_2 | 110.5 |
O3_1—Ni1_1—O5_1 | 152.60 (17) | O2_2—C2_2—H2B_2 | 110.5 |
O4_1—Ni1_1—O5_1 | 73.57 (12) | C1_2—C2_2—H2B_2 | 110.5 |
O6_1—Ni1_1—O2_1 | 92.58 (14) | H2A_2—C2_2—H2B_2 | 108.7 |
O7_1—Ni1_1—O2_1 | 78.56 (13) | O2_2—C3_2—C4_2 | 105.52 (17) |
O3_1—Ni1_1—O2_1 | 73.92 (12) | O2_2—C3_2—H3A_2 | 110.6 |
O4_1—Ni1_1—O2_1 | 150.83 (17) | C4_2—C3_2—H3A_2 | 110.6 |
O5_1—Ni1_1—O2_1 | 133.43 (15) | O2_2—C3_2—H3B_2 | 110.6 |
O6_1—Ni1_1—O1_1 | 82.10 (12) | C4_2—C3_2—H3B_2 | 110.6 |
O7_1—Ni1_1—O1_1 | 81.53 (12) | H3A_2—C3_2—H3B_2 | 108.8 |
O3_1—Ni1_1—O1_1 | 139.60 (16) | O3_2—C4_2—C3_2 | 106.45 (17) |
O4_1—Ni1_1—O1_1 | 140.26 (16) | O3_2—C4_2—H4A_2 | 110.4 |
O5_1—Ni1_1—O1_1 | 66.96 (10) | C3_2—C4_2—H4A_2 | 110.4 |
O2_1—Ni1_1—O1_1 | 66.90 (9) | O3_2—C4_2—H4B_2 | 110.4 |
O7_1—Ni1'_1—O6_1 | 171.59 (18) | C3_2—C4_2—H4B_2 | 110.4 |
O7_1—Ni1'_1—O2_1 | 86.21 (9) | H4A_2—C4_2—H4B_2 | 108.6 |
O6_1—Ni1'_1—O2_1 | 100.74 (10) | O3_2—C5_2—C6_2 | 106.24 (17) |
O7_1—Ni1'_1—O1_1 | 93.28 (11) | O3_2—C5_2—H5A_2 | 110.5 |
O6_1—Ni1'_1—O1_1 | 92.66 (11) | C6_2—C5_2—H5A_2 | 110.5 |
O2_1—Ni1'_1—O1_1 | 79.36 (12) | O3_2—C5_2—H5B_2 | 110.5 |
O7_1—Ni1'_1—O5_1 | 89.43 (8) | C6_2—C5_2—H5B_2 | 110.5 |
O6_1—Ni1'_1—O5_1 | 86.46 (8) | H5A_2—C5_2—H5B_2 | 108.7 |
O2_1—Ni1'_1—O5_1 | 152.99 (16) | O4_2—C6_2—C5_2 | 106.40 (17) |
O1_1—Ni1'_1—O5_1 | 74.29 (8) | O4_2—C6_2—H6A_2 | 110.4 |
O7_1—Ni1'_1—O3_1 | 93.88 (10) | C5_2—C6_2—H6A_2 | 110.4 |
O6_1—Ni1'_1—O3_1 | 83.56 (9) | O4_2—C6_2—H6B_2 | 110.4 |
O2_1—Ni1'_1—O3_1 | 74.46 (7) | C5_2—C6_2—H6B_2 | 110.4 |
O1_1—Ni1'_1—O3_1 | 152.30 (12) | H6A_2—C6_2—H6B_2 | 108.6 |
O5_1—Ni1'_1—O3_1 | 132.48 (15) | O4_2—C7_2—C8_2 | 106.19 (17) |
O7_1—Ni1'_1—O4_1 | 83.30 (10) | O4_2—C7_2—H7A_2 | 110.5 |
O6_1—Ni1'_1—O4_1 | 88.32 (11) | C8_2—C7_2—H7A_2 | 110.5 |
O2_1—Ni1'_1—O4_1 | 139.83 (12) | O4_2—C7_2—H7B_2 | 110.5 |
O1_1—Ni1'_1—O4_1 | 139.76 (8) | C8_2—C7_2—H7B_2 | 110.5 |
O5_1—Ni1'_1—O4_1 | 65.62 (8) | H7A_2—C7_2—H7B_2 | 108.7 |
O3_1—Ni1'_1—O4_1 | 67.75 (9) | O5_2—C8_2—C7_2 | 106.94 (17) |
C1_1—O1_1—C10_1 | 113.77 (15) | O5_2—C8_2—H8A_2 | 110.3 |
C1_1—O1_1—Ni1'_1 | 108.67 (12) | C7_2—C8_2—H8A_2 | 110.3 |
C10_1—O1_1—Ni1'_1 | 111.07 (12) | O5_2—C8_2—H8B_2 | 110.3 |
C1_1—O1_1—Ni1_1 | 112.42 (14) | C7_2—C8_2—H8B_2 | 110.3 |
C10_1—O1_1—Ni1_1 | 108.03 (13) | H8A_2—C8_2—H8B_2 | 108.6 |
C2_1—O2_1—C3_1 | 114.65 (15) | O5_2—C9_2—C10_2 | 106.50 (17) |
C2_1—O2_1—Ni1'_1 | 111.19 (14) | O5_2—C9_2—H9A_2 | 110.4 |
C3_1—O2_1—Ni1'_1 | 115.91 (14) | C10_2—C9_2—H9A_2 | 110.4 |
C2_1—O2_1—Ni1_1 | 119.38 (14) | O5_2—C9_2—H9B_2 | 110.4 |
C3_1—O2_1—Ni1_1 | 108.42 (14) | C10_2—C9_2—H9B_2 | 110.4 |
C4_1—O3_1—C5_1 | 113.87 (15) | H9A_2—C9_2—H9B_2 | 108.6 |
C4_1—O3_1—Ni1_1 | 118.21 (15) | O1_2—C10_2—C9_2 | 105.79 (17) |
C5_1—O3_1—Ni1_1 | 108.80 (14) | O1_2—C10_2—H10A_2 | 110.6 |
C4_1—O3_1—Ni1'_1 | 109.73 (13) | C9_2—C10_2—H10A_2 | 110.6 |
C5_1—O3_1—Ni1'_1 | 116.95 (13) | O1_2—C10_2—H10B_2 | 110.6 |
C7_1—O4_1—C6_1 | 114.06 (16) | C9_2—C10_2—H10B_2 | 110.6 |
C7_1—O4_1—Ni1_1 | 109.48 (15) | H10A_2—C10_2—H10B_2 | 108.7 |
C6_1—O4_1—Ni1_1 | 108.06 (15) | O7_3—Ni3_3—O6_3 | 165.41 (17) |
C7_1—O4_1—Ni1'_1 | 107.55 (12) | O7_3—Ni3_3—O3_3 | 100.25 (16) |
C6_1—O4_1—Ni1'_1 | 111.45 (12) | O6_3—Ni3_3—O3_3 | 88.35 (15) |
C8_1—O5_1—C9_1 | 114.90 (15) | O7_3—Ni3_3—O5_3 | 88.07 (15) |
C8_1—O5_1—Ni1_1 | 117.95 (14) | O6_3—Ni3_3—O5_3 | 89.62 (15) |
C9_1—O5_1—Ni1_1 | 127.12 (14) | O3_3—Ni3_3—O5_3 | 152.54 (15) |
C8_1—O5_1—Ni1'_1 | 129.13 (14) | O7_3—Ni3_3—O4_3 | 93.61 (14) |
C9_1—O5_1—Ni1'_1 | 115.95 (14) | O6_3—Ni3_3—O4_3 | 99.60 (15) |
Ni1_1—O6_1—H6W1_1 | 121.5 (15) | O3_3—Ni3_3—O4_3 | 79.26 (12) |
Ni1'_1—O6_1—H6W1_1 | 118.7 (15) | O5_3—Ni3_3—O4_3 | 74.10 (11) |
Ni1_1—O6_1—H6W2_1 | 130.1 (15) | O7_3—Ni3_3—O2_3 | 80.00 (12) |
Ni1'_1—O6_1—H6W2_1 | 130.5 (15) | O6_3—Ni3_3—O2_3 | 91.19 (13) |
H6W1_1—O6_1—H6W2_1 | 108.3 (14) | O3_3—Ni3_3—O2_3 | 74.18 (12) |
Ni1'_1—O7_1—H7W1_1 | 130.7 (15) | O5_3—Ni3_3—O2_3 | 133.25 (15) |
Ni1_1—O7_1—H7W1_1 | 127.8 (15) | O4_3—Ni3_3—O2_3 | 150.98 (18) |
Ni1'_1—O7_1—H7W2_1 | 118.1 (15) | O7_3—Ni3_3—O1_3 | 85.00 (13) |
Ni1_1—O7_1—H7W2_1 | 113.3 (15) | O6_3—Ni3_3—O1_3 | 80.84 (12) |
H7W1_1—O7_1—H7W2_1 | 105.8 (13) | O3_3—Ni3_3—O1_3 | 139.40 (14) |
O1_1—C1_1—C2_1 | 106.28 (17) | O5_3—Ni3_3—O1_3 | 66.92 (11) |
O1_1—C1_1—H1A_1 | 110.5 | O4_3—Ni3_3—O1_3 | 141.01 (17) |
C2_1—C1_1—H1A_1 | 110.5 | O2_3—Ni3_3—O1_3 | 67.12 (8) |
O1_1—C1_1—H1B_1 | 110.5 | O7_3—Ni3'_3—O6_3 | 170.26 (17) |
C2_1—C1_1—H1B_1 | 110.5 | O7_3—Ni3'_3—O2_3 | 87.54 (11) |
H1A_1—C1_1—H1B_1 | 108.7 | O6_3—Ni3'_3—O2_3 | 100.15 (12) |
O2_1—C2_1—C1_1 | 105.91 (17) | O7_3—Ni3'_3—O1_3 | 96.17 (11) |
O2_1—C2_1—H2A_1 | 110.6 | O6_3—Ni3'_3—O1_3 | 91.13 (11) |
C1_1—C2_1—H2A_1 | 110.6 | O2_3—Ni3'_3—O1_3 | 79.60 (11) |
O2_1—C2_1—H2B_1 | 110.6 | O7_3—Ni3'_3—O5_3 | 87.26 (10) |
C1_1—C2_1—H2B_1 | 110.6 | O6_3—Ni3'_3—O5_3 | 88.66 (10) |
H2A_1—C2_1—H2B_1 | 108.7 | O2_3—Ni3'_3—O5_3 | 151.83 (14) |
O2_1—C3_1—C4_1 | 105.06 (16) | O1_3—Ni3'_3—O5_3 | 73.48 (9) |
O2_1—C3_1—H3A_1 | 110.7 | O7_3—Ni3'_3—O3_3 | 93.59 (11) |
C4_1—C3_1—H3A_1 | 110.7 | O6_3—Ni3'_3—O3_3 | 82.69 (10) |
O2_1—C3_1—H3B_1 | 110.7 | O2_3—Ni3'_3—O3_3 | 75.42 (9) |
C4_1—C3_1—H3B_1 | 110.7 | O1_3—Ni3'_3—O3_3 | 152.71 (13) |
H3A_1—C3_1—H3B_1 | 108.8 | O5_3—Ni3'_3—O3_3 | 132.55 (13) |
O3_1—C4_1—C3_1 | 105.85 (16) | O7_3—Ni3'_3—O4_3 | 82.65 (11) |
O3_1—C4_1—H4A_1 | 110.6 | O6_3—Ni3'_3—O4_3 | 87.61 (11) |
C3_1—C4_1—H4A_1 | 110.6 | O2_3—Ni3'_3—O4_3 | 140.65 (12) |
O3_1—C4_1—H4B_1 | 110.6 | O1_3—Ni3'_3—O4_3 | 139.21 (11) |
C3_1—C4_1—H4B_1 | 110.6 | O5_3—Ni3'_3—O4_3 | 65.74 (8) |
H4A_1—C4_1—H4B_1 | 108.7 | O3_3—Ni3'_3—O4_3 | 67.35 (8) |
O3_1—C5_1—C6_1 | 106.10 (17) | C10_3—O1_3—C1_3 | 113.49 (16) |
O3_1—C5_1—H5A_1 | 110.5 | C10_3—O1_3—Ni3'_3 | 112.18 (13) |
C6_1—C5_1—H5A_1 | 110.5 | C1_3—O1_3—Ni3'_3 | 107.91 (13) |
O3_1—C5_1—H5B_1 | 110.5 | C10_3—O1_3—Ni3_3 | 108.64 (14) |
C6_1—C5_1—H5B_1 | 110.5 | C1_3—O1_3—Ni3_3 | 112.06 (14) |
H5A_1—C5_1—H5B_1 | 108.7 | C3_3—O2_3—C2_3 | 113.89 (15) |
O4_1—C6_1—C5_1 | 106.02 (17) | C3_3—O2_3—Ni3'_3 | 116.15 (14) |
O4_1—C6_1—H6A_1 | 110.5 | C2_3—O2_3—Ni3'_3 | 111.98 (14) |
C5_1—C6_1—H6A_1 | 110.5 | C3_3—O2_3—Ni3_3 | 109.16 (15) |
O4_1—C6_1—H6B_1 | 110.5 | C2_3—O2_3—Ni3_3 | 119.79 (14) |
C5_1—C6_1—H6B_1 | 110.5 | C4_3—O3_3—C5_3 | 114.28 (16) |
H6A_1—C6_1—H6B_1 | 108.7 | C4_3—O3_3—Ni3_3 | 117.29 (14) |
O4_1—C7_1—C8_1 | 106.28 (17) | C5_3—O3_3—Ni3_3 | 110.74 (14) |
O4_1—C7_1—H7A_1 | 110.5 | C4_3—O3_3—Ni3'_3 | 108.92 (13) |
C8_1—C7_1—H7A_1 | 110.5 | C5_3—O3_3—Ni3'_3 | 119.53 (14) |
O4_1—C7_1—H7B_1 | 110.5 | C7_3—O4_3—C6_3 | 113.94 (16) |
C8_1—C7_1—H7B_1 | 110.5 | C7_3—O4_3—Ni3_3 | 109.29 (15) |
H7A_1—C7_1—H7B_1 | 108.7 | C6_3—O4_3—Ni3_3 | 108.08 (15) |
O5_1—C8_1—C7_1 | 106.28 (16) | C7_3—O4_3—Ni3'_3 | 107.46 (13) |
O5_1—C8_1—H8A_1 | 110.5 | C6_3—O4_3—Ni3'_3 | 110.63 (13) |
C7_1—C8_1—H8A_1 | 110.5 | C8_3—O5_3—C9_3 | 115.37 (15) |
O5_1—C8_1—H8B_1 | 110.5 | C8_3—O5_3—Ni3_3 | 117.23 (14) |
C7_1—C8_1—H8B_1 | 110.5 | C9_3—O5_3—Ni3_3 | 126.98 (14) |
H8A_1—C8_1—H8B_1 | 108.7 | C8_3—O5_3—Ni3'_3 | 128.13 (14) |
O5_1—C9_1—C10_1 | 106.66 (16) | C9_3—O5_3—Ni3'_3 | 116.11 (13) |
O5_1—C9_1—H9A_1 | 110.4 | Ni3'_3—O6_3—H6W1_3 | 121.3 (14) |
C10_1—C9_1—H9A_1 | 110.4 | Ni3_3—O6_3—H6W1_3 | 122.1 (14) |
O5_1—C9_1—H9B_1 | 110.4 | Ni3'_3—O6_3—H6W2_3 | 131.2 (14) |
C10_1—C9_1—H9B_1 | 110.4 | Ni3_3—O6_3—H6W2_3 | 126.5 (15) |
H9A_1—C9_1—H9B_1 | 108.6 | H6W1_3—O6_3—H6W2_3 | 106.8 (13) |
O1_1—C10_1—C9_1 | 104.77 (16) | Ni3'_3—O7_3—H7W1_3 | 128.7 (15) |
O1_1—C10_1—H10A_1 | 110.8 | Ni3_3—O7_3—H7W1_3 | 128.3 (16) |
C9_1—C10_1—H10A_1 | 110.8 | Ni3'_3—O7_3—H7W2_3 | 120.8 (15) |
O1_1—C10_1—H10B_1 | 110.8 | Ni3_3—O7_3—H7W2_3 | 115.8 (16) |
C9_1—C10_1—H10B_1 | 110.8 | H7W1_3—O7_3—H7W2_3 | 108.3 (14) |
H10A_1—C10_1—H10B_1 | 108.9 | O1_3—C1_3—C2_3 | 106.33 (18) |
O6_2—Ni2_2—O7_2 | 166.58 (16) | O1_3—C1_3—H1A_3 | 110.5 |
O6_2—Ni2_2—O3_2 | 88.44 (14) | C2_3—C1_3—H1A_3 | 110.5 |
O7_2—Ni2_2—O3_2 | 100.37 (15) | O1_3—C1_3—H1B_3 | 110.5 |
O6_2—Ni2_2—O4_2 | 97.27 (13) | C2_3—C1_3—H1B_3 | 110.5 |
O7_2—Ni2_2—O4_2 | 94.26 (13) | H1A_3—C1_3—H1B_3 | 108.7 |
O3_2—Ni2_2—O4_2 | 79.87 (11) | O2_3—C2_3—C1_3 | 105.71 (17) |
O6_2—Ni2_2—O5_2 | 88.26 (14) | O2_3—C2_3—H2A_3 | 110.6 |
O7_2—Ni2_2—O5_2 | 88.28 (14) | C1_3—C2_3—H2A_3 | 110.6 |
O3_2—Ni2_2—O5_2 | 153.25 (14) | O2_3—C2_3—H2B_3 | 110.6 |
O4_2—Ni2_2—O5_2 | 74.24 (11) | C1_3—C2_3—H2B_3 | 110.6 |
O6_2—Ni2_2—O2_2 | 94.23 (12) | H2A_3—C2_3—H2B_3 | 108.7 |
O7_2—Ni2_2—O2_2 | 78.97 (11) | O2_3—C3_3—C4_3 | 105.10 (16) |
O3_2—Ni2_2—O2_2 | 72.69 (11) | O2_3—C3_3—H3A_3 | 110.7 |
O4_2—Ni2_2—O2_2 | 149.87 (17) | C4_3—C3_3—H3A_3 | 110.7 |
O5_2—Ni2_2—O2_2 | 134.04 (14) | O2_3—C3_3—H3B_3 | 110.7 |
O6_2—Ni2_2—O1_2 | 82.99 (11) | C4_3—C3_3—H3B_3 | 110.7 |
O7_2—Ni2_2—O1_2 | 83.69 (11) | H3A_3—C3_3—H3B_3 | 108.8 |
O3_2—Ni2_2—O1_2 | 137.78 (14) | O3_3—C4_3—C3_3 | 106.01 (17) |
O4_2—Ni2_2—O1_2 | 142.16 (17) | O3_3—C4_3—H4A_3 | 110.5 |
O5_2—Ni2_2—O1_2 | 67.94 (10) | C3_3—C4_3—H4A_3 | 110.5 |
O2_2—Ni2_2—O1_2 | 66.87 (8) | O3_3—C4_3—H4B_3 | 110.5 |
O7_2—Ni2'_2—O6_2 | 168.35 (16) | C3_3—C4_3—H4B_3 | 110.5 |
O7_2—Ni2'_2—O2_2 | 86.13 (11) | H4A_3—C4_3—H4B_3 | 108.7 |
O6_2—Ni2'_2—O2_2 | 102.66 (12) | O3_3—C5_3—C6_3 | 106.25 (18) |
O7_2—Ni2'_2—O1_2 | 95.35 (11) | O3_3—C5_3—H5A_3 | 110.5 |
O6_2—Ni2'_2—O1_2 | 93.80 (12) | C6_3—C5_3—H5A_3 | 110.5 |
O2_2—Ni2'_2—O1_2 | 79.40 (10) | O3_3—C5_3—H5B_3 | 110.5 |
O7_2—Ni2'_2—O5_2 | 88.00 (11) | C6_3—C5_3—H5B_3 | 110.5 |
O6_2—Ni2'_2—O5_2 | 87.35 (11) | H5A_3—C5_3—H5B_3 | 108.7 |
O2_2—Ni2'_2—O5_2 | 153.42 (14) | O4_3—C6_3—C5_3 | 106.27 (18) |
O1_2—Ni2'_2—O5_2 | 75.37 (10) | O4_3—C6_3—H6A_3 | 110.5 |
O7_2—Ni2'_2—O3_2 | 93.38 (11) | C5_3—C6_3—H6A_3 | 110.5 |
O6_2—Ni2'_2—O3_2 | 82.05 (10) | O4_3—C6_3—H6B_3 | 110.5 |
O2_2—Ni2'_2—O3_2 | 73.33 (9) | C5_3—C6_3—H6B_3 | 110.5 |
O1_2—Ni2'_2—O3_2 | 150.68 (14) | H6A_3—C6_3—H6B_3 | 108.7 |
O5_2—Ni2'_2—O3_2 | 132.96 (13) | O4_3—C7_3—C8_3 | 106.37 (17) |
O7_2—Ni2'_2—O4_2 | 83.16 (10) | O4_3—C7_3—H7A_3 | 110.5 |
O6_2—Ni2'_2—O4_2 | 85.18 (10) | C8_3—C7_3—H7A_3 | 110.5 |
O2_2—Ni2'_2—O4_2 | 138.65 (12) | O4_3—C7_3—H7B_3 | 110.5 |
O1_2—Ni2'_2—O4_2 | 141.26 (13) | C8_3—C7_3—H7B_3 | 110.5 |
O5_2—Ni2'_2—O4_2 | 65.90 (9) | H7A_3—C7_3—H7B_3 | 108.6 |
O3_2—Ni2'_2—O4_2 | 67.61 (8) | O5_3—C8_3—C7_3 | 106.99 (17) |
C10_2—O1_2—C1_2 | 112.98 (16) | O5_3—C8_3—H8A_3 | 110.3 |
C10_2—O1_2—Ni2'_2 | 110.98 (14) | C7_3—C8_3—H8A_3 | 110.3 |
C1_2—O1_2—Ni2'_2 | 108.80 (14) | O5_3—C8_3—H8B_3 | 110.3 |
C10_2—O1_2—Ni2_2 | 107.73 (14) | C7_3—C8_3—H8B_3 | 110.3 |
C1_2—O1_2—Ni2_2 | 112.46 (14) | H8A_3—C8_3—H8B_3 | 108.6 |
C2_2—O2_2—C3_2 | 114.27 (15) | O5_3—C9_3—C10_3 | 106.89 (16) |
C2_2—O2_2—Ni2'_2 | 111.15 (14) | O5_3—C9_3—H9A_3 | 110.3 |
C3_2—O2_2—Ni2'_2 | 117.82 (14) | C10_3—C9_3—H9A_3 | 110.3 |
C2_2—O2_2—Ni2_2 | 119.51 (14) | O5_3—C9_3—H9B_3 | 110.3 |
C3_2—O2_2—Ni2_2 | 110.44 (14) | C10_3—C9_3—H9B_3 | 110.3 |
C4_2—O3_2—C5_2 | 113.78 (15) | H9A_3—C9_3—H9B_3 | 108.6 |
C4_2—O3_2—Ni2_2 | 118.54 (14) | O1_3—C10_3—C9_3 | 104.99 (16) |
C5_2—O3_2—Ni2_2 | 108.12 (14) | O1_3—C10_3—H10A_3 | 110.7 |
C4_2—O3_2—Ni2'_2 | 110.26 (13) | C9_3—C10_3—H10A_3 | 110.7 |
C5_2—O3_2—Ni2'_2 | 116.68 (13) | O1_3—C10_3—H10B_3 | 110.7 |
C7_2—O4_2—C6_2 | 114.03 (16) | C9_3—C10_3—H10B_3 | 110.7 |
C7_2—O4_2—Ni2_2 | 110.10 (15) | H10A_3—C10_3—H10B_3 | 108.8 |
C6_2—O4_2—Ni2_2 | 108.74 (15) | O10_4—N1_4—O8_4 | 121.15 (19) |
C7_2—O4_2—Ni2'_2 | 107.94 (13) | O10_4—N1_4—O9_4 | 120.25 (19) |
C6_2—O4_2—Ni2'_2 | 111.73 (13) | O8_4—N1_4—O9_4 | 118.58 (17) |
C9_2—O5_2—C8_2 | 115.77 (15) | O10_5—N2_5—O9_5 | 121.13 (19) |
C9_2—O5_2—Ni2_2 | 126.29 (13) | O10_5—N2_5—O8_5 | 120.69 (19) |
C8_2—O5_2—Ni2_2 | 117.38 (14) | O9_5—N2_5—O8_5 | 118.17 (17) |
C9_2—O5_2—Ni2'_2 | 114.99 (13) | O10_6—N3_6—O8_6 | 121.59 (19) |
C8_2—O5_2—Ni2'_2 | 128.67 (14) | O10_6—N3_6—O9_6 | 119.32 (18) |
Ni2_2—O6_2—H6W1_2 | 120.2 (15) | O8_6—N3_6—O9_6 | 119.08 (19) |
Ni2'_2—O6_2—H6W1_2 | 116.9 (16) | O10_7—N4_7—O8_7 | 121.52 (19) |
Ni2_2—O6_2—H6W2_2 | 123.8 (15) | O10_7—N4_7—O9_7 | 119.68 (19) |
Ni2'_2—O6_2—H6W2_2 | 118.1 (16) | O8_7—N4_7—O9_7 | 118.78 (19) |
H6W1_2—O6_2—H6W2_2 | 107.0 (14) | O10_8—N5_8—O8_8 | 120.97 (18) |
Ni2'_2—O7_2—H7W1_2 | 121.7 (15) | O10_8—N5_8—O9_8 | 120.34 (18) |
Ni2_2—O7_2—H7W1_2 | 114.8 (15) | O8_8—N5_8—O9_8 | 118.67 (17) |
Ni2'_2—O7_2—H7W2_2 | 126.6 (15) | O10_9—N6_9—O9_9 | 120.56 (18) |
Ni2_2—O7_2—H7W2_2 | 125.7 (15) | O10_9—N6_9—O8_9 | 120.96 (19) |
H7W1_2—O7_2—H7W2_2 | 105.6 (13) | O9_9—N6_9—O8_9 | 118.47 (18) |
O1_2—C1_2—C2_2 | 106.27 (17) | | |
| | | |
O7_1—Ni1'_1—O1_1—C1_1 | 68.66 (14) | O6_2—Ni2_2—O4_2—Ni2'_2 | 96 (3) |
O6_1—Ni1'_1—O1_1—C1_1 | −117.30 (14) | O7_2—Ni2_2—O4_2—Ni2'_2 | −77 (3) |
O2_1—Ni1'_1—O1_1—C1_1 | −16.86 (13) | O3_2—Ni2_2—O4_2—Ni2'_2 | −176 (3) |
O5_1—Ni1'_1—O1_1—C1_1 | 157.14 (13) | O5_2—Ni2_2—O4_2—Ni2'_2 | 10 (3) |
O3_1—Ni1'_1—O1_1—C1_1 | −36.1 (3) | O2_2—Ni2_2—O4_2—Ni2'_2 | −152 (3) |
O4_1—Ni1'_1—O1_1—C1_1 | 152.16 (14) | O1_2—Ni2_2—O4_2—Ni2'_2 | 9 (2) |
O7_1—Ni1'_1—O1_1—C10_1 | −57.23 (15) | O7_2—Ni2'_2—O4_2—C7_2 | −124.27 (14) |
O6_1—Ni1'_1—O1_1—C10_1 | 116.82 (14) | O6_2—Ni2'_2—O4_2—C7_2 | 55.84 (14) |
O2_1—Ni1'_1—O1_1—C10_1 | −142.75 (13) | O2_2—Ni2'_2—O4_2—C7_2 | 159.56 (18) |
O5_1—Ni1'_1—O1_1—C10_1 | 31.25 (13) | O1_2—Ni2'_2—O4_2—C7_2 | −34.2 (2) |
O3_1—Ni1'_1—O1_1—C10_1 | −161.99 (19) | O5_2—Ni2'_2—O4_2—C7_2 | −33.40 (13) |
O4_1—Ni1'_1—O1_1—C10_1 | 26.3 (2) | O3_2—Ni2'_2—O4_2—C7_2 | 139.21 (13) |
O7_1—Ni1'_1—O1_1—Ni1_1 | −96.1 (17) | O7_2—Ni2'_2—O4_2—C6_2 | 109.59 (15) |
O6_1—Ni1'_1—O1_1—Ni1_1 | 77.9 (17) | O6_2—Ni2'_2—O4_2—C6_2 | −70.30 (15) |
O2_1—Ni1'_1—O1_1—Ni1_1 | 178.3 (17) | O2_2—Ni2'_2—O4_2—C6_2 | 33.4 (2) |
O5_1—Ni1'_1—O1_1—Ni1_1 | −7.7 (17) | O1_2—Ni2'_2—O4_2—C6_2 | −160.37 (19) |
O3_1—Ni1'_1—O1_1—Ni1_1 | 159.1 (19) | O5_2—Ni2'_2—O4_2—C6_2 | −159.54 (14) |
O4_1—Ni1'_1—O1_1—Ni1_1 | −12.6 (16) | O3_2—Ni2'_2—O4_2—C6_2 | 13.07 (14) |
O6_1—Ni1_1—O1_1—C1_1 | −113.39 (15) | O7_2—Ni2'_2—O4_2—Ni2_2 | 100 (3) |
O7_1—Ni1_1—O1_1—C1_1 | 63.95 (16) | O6_2—Ni2'_2—O4_2—Ni2_2 | −80 (3) |
O3_1—Ni1_1—O1_1—C1_1 | −32.2 (3) | O2_2—Ni2'_2—O4_2—Ni2_2 | 24 (2) |
O4_1—Ni1_1—O1_1—C1_1 | 149.2 (2) | O1_2—Ni2'_2—O4_2—Ni2_2 | −170 (3) |
O5_1—Ni1_1—O1_1—C1_1 | 156.33 (14) | O5_2—Ni2'_2—O4_2—Ni2_2 | −169 (3) |
O2_1—Ni1_1—O1_1—C1_1 | −17.16 (15) | O3_2—Ni2'_2—O4_2—Ni2_2 | 3 (3) |
O6_1—Ni1_1—O1_1—C10_1 | 120.25 (15) | O6_2—Ni2_2—O5_2—C9_2 | 80.67 (19) |
O7_1—Ni1_1—O1_1—C10_1 | −62.41 (16) | O7_2—Ni2_2—O5_2—C9_2 | −86.36 (19) |
O3_1—Ni1_1—O1_1—C10_1 | −158.6 (2) | O3_2—Ni2_2—O5_2—C9_2 | 163.7 (3) |
O4_1—Ni1_1—O1_1—C10_1 | 22.9 (3) | O4_2—Ni2_2—O5_2—C9_2 | 178.72 (16) |
O5_1—Ni1_1—O1_1—C10_1 | 29.97 (15) | O2_2—Ni2_2—O5_2—C9_2 | −13.5 (3) |
O2_1—Ni1_1—O1_1—C10_1 | −143.52 (14) | O1_2—Ni2_2—O5_2—C9_2 | −2.47 (18) |
O6_1—Ni1_1—O1_1—Ni1'_1 | −97.8 (17) | O6_2—Ni2_2—O5_2—C8_2 | −90.31 (16) |
O7_1—Ni1_1—O1_1—Ni1'_1 | 79.5 (17) | O7_2—Ni2_2—O5_2—C8_2 | 102.66 (16) |
O3_1—Ni1_1—O1_1—Ni1'_1 | −16.6 (15) | O3_2—Ni2_2—O5_2—C8_2 | −7.2 (4) |
O4_1—Ni1_1—O1_1—Ni1'_1 | 164.8 (19) | O4_2—Ni2_2—O5_2—C8_2 | 7.74 (17) |
O5_1—Ni1_1—O1_1—Ni1'_1 | 171.9 (18) | O2_2—Ni2_2—O5_2—C8_2 | 175.49 (19) |
O2_1—Ni1_1—O1_1—Ni1'_1 | −1.6 (17) | O1_2—Ni2_2—O5_2—C8_2 | −173.45 (15) |
O7_1—Ni1'_1—O2_1—C2_1 | −109.88 (15) | O6_2—Ni2_2—O5_2—Ni2'_2 | 85.2 (7) |
O6_1—Ni1'_1—O2_1—C2_1 | 74.89 (17) | O7_2—Ni2_2—O5_2—Ni2'_2 | −81.8 (7) |
O1_1—Ni1'_1—O2_1—C2_1 | −15.82 (13) | O3_2—Ni2_2—O5_2—Ni2'_2 | 168.3 (11) |
O5_1—Ni1'_1—O2_1—C2_1 | −28.6 (3) | O4_2—Ni2_2—O5_2—Ni2'_2 | −176.7 (8) |
O3_1—Ni1'_1—O2_1—C2_1 | 155.03 (14) | O2_2—Ni2_2—O5_2—Ni2'_2 | −9.0 (5) |
O4_1—Ni1'_1—O2_1—C2_1 | 175.18 (14) | O1_2—Ni2_2—O5_2—Ni2'_2 | 2.1 (7) |
O7_1—Ni1'_1—O2_1—C3_1 | 116.83 (15) | O7_2—Ni2'_2—O5_2—C9_2 | −97.74 (16) |
O6_1—Ni1'_1—O2_1—C3_1 | −58.40 (18) | O6_2—Ni2'_2—O5_2—C9_2 | 92.94 (15) |
O1_1—Ni1'_1—O2_1—C3_1 | −149.11 (14) | O2_2—Ni2'_2—O5_2—C9_2 | −20.5 (4) |
O5_1—Ni1'_1—O2_1—C3_1 | −161.9 (2) | O1_2—Ni2'_2—O5_2—C9_2 | −1.68 (15) |
O3_1—Ni1'_1—O2_1—C3_1 | 21.74 (14) | O3_2—Ni2'_2—O5_2—C9_2 | 169.50 (16) |
O4_1—Ni1'_1—O2_1—C3_1 | 41.9 (2) | O4_2—Ni2'_2—O5_2—C9_2 | 178.85 (14) |
O7_1—Ni1'_1—O2_1—Ni1_1 | 86.8 (8) | O7_2—Ni2'_2—O5_2—C8_2 | 91.39 (18) |
O6_1—Ni1'_1—O2_1—Ni1_1 | −88.5 (8) | O6_2—Ni2'_2—O5_2—C8_2 | −77.92 (19) |
O1_1—Ni1'_1—O2_1—Ni1_1 | −179.2 (9) | O2_2—Ni2'_2—O5_2—C8_2 | 168.6 (3) |
O5_1—Ni1'_1—O2_1—Ni1_1 | 168.0 (10) | O1_2—Ni2'_2—O5_2—C8_2 | −172.55 (17) |
O3_1—Ni1'_1—O2_1—Ni1_1 | −8.3 (8) | O3_2—Ni2'_2—O5_2—C8_2 | −1.4 (3) |
O4_1—Ni1'_1—O2_1—Ni1_1 | 11.8 (7) | O4_2—Ni2'_2—O5_2—C8_2 | 7.99 (17) |
O6_1—Ni1_1—O2_1—C2_1 | 63.18 (18) | O7_2—Ni2'_2—O5_2—Ni2_2 | 86.3 (7) |
O7_1—Ni1_1—O2_1—C2_1 | −102.68 (16) | O6_2—Ni2'_2—O5_2—Ni2_2 | −83.0 (7) |
O3_1—Ni1_1—O2_1—C2_1 | 152.82 (15) | O2_2—Ni2'_2—O5_2—Ni2_2 | 163.5 (10) |
O4_1—Ni1_1—O2_1—C2_1 | −179.1 (3) | O1_2—Ni2'_2—O5_2—Ni2_2 | −177.6 (8) |
O5_1—Ni1_1—O2_1—C2_1 | −25.4 (3) | O3_2—Ni2'_2—O5_2—Ni2_2 | −6.5 (6) |
O1_1—Ni1_1—O2_1—C2_1 | −17.10 (16) | O4_2—Ni2'_2—O5_2—Ni2_2 | 2.9 (7) |
O6_1—Ni1_1—O2_1—C3_1 | −70.62 (16) | O7_2—Ni2_2—O6_2—Ni2'_2 | −12.6 (3) |
O7_1—Ni1_1—O2_1—C3_1 | 123.52 (15) | O3_2—Ni2_2—O6_2—Ni2'_2 | 118.7 (8) |
O3_1—Ni1_1—O2_1—C3_1 | 19.02 (16) | O4_2—Ni2_2—O6_2—Ni2'_2 | −161.7 (9) |
O4_1—Ni1_1—O2_1—C3_1 | 47.1 (4) | O5_2—Ni2_2—O6_2—Ni2'_2 | −87.8 (8) |
O5_1—Ni1_1—O2_1—C3_1 | −159.2 (2) | O2_2—Ni2_2—O6_2—Ni2'_2 | 46.2 (7) |
O1_1—Ni1_1—O2_1—C3_1 | −150.90 (13) | O1_2—Ni2_2—O6_2—Ni2'_2 | −19.8 (7) |
O6_1—Ni1_1—O2_1—Ni1'_1 | 81.0 (8) | O7_2—Ni2'_2—O6_2—Ni2_2 | 14.7 (4) |
O7_1—Ni1_1—O2_1—Ni1'_1 | −84.8 (8) | O2_2—Ni2'_2—O6_2—Ni2_2 | −123.6 (8) |
O3_1—Ni1_1—O2_1—Ni1'_1 | 170.7 (9) | O1_2—Ni2'_2—O6_2—Ni2_2 | 156.4 (9) |
O4_1—Ni1_1—O2_1—Ni1'_1 | −161.3 (11) | O5_2—Ni2'_2—O6_2—Ni2_2 | 81.3 (8) |
O5_1—Ni1_1—O2_1—Ni1'_1 | −7.5 (6) | O3_2—Ni2'_2—O6_2—Ni2_2 | −52.8 (8) |
O1_1—Ni1_1—O2_1—Ni1'_1 | 0.7 (8) | O4_2—Ni2'_2—O6_2—Ni2_2 | 15.2 (7) |
O6_1—Ni1_1—O3_1—C4_1 | 107.00 (17) | O6_2—Ni2'_2—O7_2—Ni2_2 | −14.6 (4) |
O7_1—Ni1_1—O3_1—C4_1 | −60.34 (19) | O2_2—Ni2'_2—O7_2—Ni2_2 | 124.8 (8) |
O4_1—Ni1_1—O3_1—C4_1 | −152.12 (14) | O1_2—Ni2'_2—O7_2—Ni2_2 | −156.2 (9) |
O5_1—Ni1_1—O3_1—C4_1 | −168.5 (4) | O5_2—Ni2'_2—O7_2—Ni2_2 | −81.1 (8) |
O2_1—Ni1_1—O3_1—C4_1 | 14.42 (17) | O3_2—Ni2'_2—O7_2—Ni2_2 | 51.8 (7) |
O1_1—Ni1_1—O3_1—C4_1 | 28.8 (3) | O4_2—Ni2'_2—O7_2—Ni2_2 | −15.1 (7) |
O6_1—Ni1_1—O3_1—C5_1 | −121.12 (16) | O6_2—Ni2_2—O7_2—Ni2'_2 | 12.7 (3) |
O7_1—Ni1_1—O3_1—C5_1 | 71.54 (18) | O3_2—Ni2_2—O7_2—Ni2'_2 | −117.6 (8) |
O4_1—Ni1_1—O3_1—C5_1 | −20.24 (17) | O4_2—Ni2_2—O7_2—Ni2'_2 | 161.9 (9) |
O5_1—Ni1_1—O3_1—C5_1 | −36.6 (4) | O5_2—Ni2_2—O7_2—Ni2'_2 | 87.9 (8) |
O2_1—Ni1_1—O3_1—C5_1 | 146.30 (14) | O2_2—Ni2_2—O7_2—Ni2'_2 | −47.7 (7) |
O1_1—Ni1_1—O3_1—C5_1 | 160.7 (2) | O1_2—Ni2_2—O7_2—Ni2'_2 | 19.9 (7) |
O6_1—Ni1_1—O3_1—Ni1'_1 | 84.7 (8) | C10_2—O1_2—C1_2—C2_2 | −169.30 (17) |
O7_1—Ni1_1—O3_1—Ni1'_1 | −82.6 (8) | Ni2'_2—O1_2—C1_2—C2_2 | −45.6 (2) |
O4_1—Ni1_1—O3_1—Ni1'_1 | −174.4 (9) | Ni2_2—O1_2—C1_2—C2_2 | −47.1 (2) |
O5_1—Ni1_1—O3_1—Ni1'_1 | 169.2 (12) | C3_2—O2_2—C2_2—C1_2 | −179.09 (17) |
O2_1—Ni1_1—O3_1—Ni1'_1 | −7.9 (8) | Ni2'_2—O2_2—C2_2—C1_2 | −42.8 (2) |
O1_1—Ni1_1—O3_1—Ni1'_1 | 6.5 (6) | Ni2_2—O2_2—C2_2—C1_2 | −45.0 (2) |
O7_1—Ni1'_1—O3_1—C4_1 | −73.04 (15) | O1_2—C1_2—C2_2—O2_2 | 58.2 (2) |
O6_1—Ni1'_1—O3_1—C4_1 | 115.00 (14) | C2_2—O2_2—C3_2—C4_2 | −178.87 (17) |
O2_1—Ni1'_1—O3_1—C4_1 | 11.93 (13) | Ni2'_2—O2_2—C3_2—C4_2 | 47.9 (2) |
O1_1—Ni1'_1—O3_1—C4_1 | 31.6 (3) | Ni2_2—O2_2—C3_2—C4_2 | 43.0 (2) |
O5_1—Ni1'_1—O3_1—C4_1 | −165.82 (14) | C5_2—O3_2—C4_2—C3_2 | 173.36 (17) |
O4_1—Ni1'_1—O3_1—C4_1 | −154.18 (13) | Ni2_2—O3_2—C4_2—C3_2 | 44.6 (2) |
O7_1—Ni1'_1—O3_1—C5_1 | 58.60 (17) | Ni2'_2—O3_2—C4_2—C3_2 | 40.06 (19) |
O6_1—Ni1'_1—O3_1—C5_1 | −113.36 (16) | O2_2—C3_2—C4_2—O3_2 | −55.3 (2) |
O2_1—Ni1'_1—O3_1—C5_1 | 143.57 (15) | C4_2—O3_2—C5_2—C6_2 | 177.47 (16) |
O1_1—Ni1'_1—O3_1—C5_1 | 163.2 (2) | Ni2_2—O3_2—C5_2—C6_2 | −48.6 (2) |
O5_1—Ni1'_1—O3_1—C5_1 | −34.17 (19) | Ni2'_2—O3_2—C5_2—C6_2 | −52.4 (2) |
O4_1—Ni1'_1—O3_1—C5_1 | −22.53 (14) | C7_2—O4_2—C6_2—C5_2 | −165.64 (17) |
O7_1—Ni1'_1—O3_1—Ni1_1 | 86.1 (8) | Ni2_2—O4_2—C6_2—C5_2 | −42.4 (2) |
O6_1—Ni1'_1—O3_1—Ni1_1 | −85.8 (8) | Ni2'_2—O4_2—C6_2—C5_2 | −42.9 (2) |
O2_1—Ni1'_1—O3_1—Ni1_1 | 171.1 (9) | O3_2—C5_2—C6_2—O4_2 | 61.0 (2) |
O1_1—Ni1'_1—O3_1—Ni1_1 | −169.2 (10) | C6_2—O4_2—C7_2—C8_2 | 177.41 (17) |
O5_1—Ni1'_1—O3_1—Ni1_1 | −6.6 (7) | Ni2_2—O4_2—C7_2—C8_2 | 54.9 (2) |
O4_1—Ni1'_1—O3_1—Ni1_1 | 5.0 (8) | Ni2'_2—O4_2—C7_2—C8_2 | 52.63 (18) |
O6_1—Ni1_1—O4_1—C7_1 | −49.31 (19) | C9_2—O5_2—C8_2—C7_2 | −153.52 (17) |
O7_1—Ni1_1—O4_1—C7_1 | 122.23 (16) | Ni2_2—O5_2—C8_2—C7_2 | 18.4 (2) |
O3_1—Ni1_1—O4_1—C7_1 | −137.79 (14) | Ni2'_2—O5_2—C8_2—C7_2 | 17.3 (3) |
O5_1—Ni1_1—O4_1—C7_1 | 34.46 (15) | O4_2—C7_2—C8_2—O5_2 | −46.2 (2) |
O2_1—Ni1_1—O4_1—C7_1 | −165.1 (3) | C8_2—O5_2—C9_2—C10_2 | −158.43 (17) |
O1_1—Ni1_1—O4_1—C7_1 | 41.3 (3) | Ni2_2—O5_2—C9_2—C10_2 | 30.5 (2) |
O6_1—Ni1_1—O4_1—C6_1 | 75.46 (18) | Ni2'_2—O5_2—C9_2—C10_2 | 29.5 (2) |
O7_1—Ni1_1—O4_1—C6_1 | −113.00 (16) | C1_2—O1_2—C10_2—C9_2 | 175.56 (17) |
O3_1—Ni1_1—O4_1—C6_1 | −13.02 (17) | Ni2'_2—O1_2—C10_2—C9_2 | 53.1 (2) |
O5_1—Ni1_1—O4_1—C6_1 | 159.22 (15) | Ni2_2—O1_2—C10_2—C9_2 | 50.7 (2) |
O2_1—Ni1_1—O4_1—C6_1 | −40.3 (4) | O5_2—C9_2—C10_2—O1_2 | −52.3 (2) |
O1_1—Ni1_1—O4_1—C6_1 | 166.0 (2) | O7_3—Ni3'_3—O1_3—C10_3 | 55.95 (16) |
O6_1—Ni1_1—O4_1—Ni1'_1 | −105 (2) | O6_3—Ni3'_3—O1_3—C10_3 | −117.60 (15) |
O7_1—Ni1_1—O4_1—Ni1'_1 | 66 (2) | O2_3—Ni3'_3—O1_3—C10_3 | 142.29 (14) |
O3_1—Ni1_1—O4_1—Ni1'_1 | 166 (2) | O5_3—Ni3'_3—O1_3—C10_3 | −29.33 (14) |
O5_1—Ni1_1—O4_1—Ni1'_1 | −21 (2) | O3_3—Ni3'_3—O1_3—C10_3 | 166.2 (2) |
O2_1—Ni1_1—O4_1—Ni1'_1 | 139 (2) | O4_3—Ni3'_3—O1_3—C10_3 | −29.9 (2) |
O1_1—Ni1_1—O4_1—Ni1'_1 | −14.5 (19) | O7_3—Ni3'_3—O1_3—C1_3 | −69.79 (16) |
O7_1—Ni1'_1—O4_1—C7_1 | 124.94 (13) | O6_3—Ni3'_3—O1_3—C1_3 | 116.67 (14) |
O6_1—Ni1'_1—O4_1—C7_1 | −54.35 (14) | O2_3—Ni3'_3—O1_3—C1_3 | 16.56 (14) |
O2_1—Ni1'_1—O4_1—C7_1 | −159.09 (15) | O5_3—Ni3'_3—O1_3—C1_3 | −155.07 (14) |
O1_1—Ni1'_1—O4_1—C7_1 | 37.79 (19) | O3_3—Ni3'_3—O1_3—C1_3 | 40.5 (3) |
O5_1—Ni1'_1—O4_1—C7_1 | 32.52 (12) | O4_3—Ni3'_3—O1_3—C1_3 | −155.67 (17) |
O3_1—Ni1'_1—O4_1—C7_1 | −138.07 (13) | O7_3—Ni3'_3—O1_3—Ni3_3 | 92.3 (18) |
O7_1—Ni1'_1—O4_1—C6_1 | −109.35 (15) | O6_3—Ni3'_3—O1_3—Ni3_3 | −81.2 (17) |
O6_1—Ni1'_1—O4_1—C6_1 | 71.36 (15) | O2_3—Ni3'_3—O1_3—Ni3_3 | 178.7 (18) |
O2_1—Ni1'_1—O4_1—C6_1 | −33.4 (2) | O5_3—Ni3'_3—O1_3—Ni3_3 | 7.0 (17) |
O1_1—Ni1'_1—O4_1—C6_1 | 163.50 (15) | O3_3—Ni3'_3—O1_3—Ni3_3 | −157 (2) |
O5_1—Ni1'_1—O4_1—C6_1 | 158.24 (15) | O4_3—Ni3'_3—O1_3—Ni3_3 | 6.4 (16) |
O3_1—Ni1'_1—O4_1—C6_1 | −12.36 (13) | O7_3—Ni3_3—O1_3—C10_3 | 62.08 (16) |
O7_1—Ni1'_1—O4_1—Ni1_1 | −110 (2) | O6_3—Ni3_3—O1_3—C10_3 | −121.46 (15) |
O6_1—Ni1'_1—O4_1—Ni1_1 | 71 (2) | O3_3—Ni3_3—O1_3—C10_3 | 162.0 (2) |
O2_1—Ni1'_1—O4_1—Ni1_1 | −34 (2) | O5_3—Ni3_3—O1_3—C10_3 | −27.95 (15) |
O1_1—Ni1'_1—O4_1—Ni1_1 | 163 (2) | O4_3—Ni3_3—O1_3—C10_3 | −27.5 (3) |
O5_1—Ni1'_1—O4_1—Ni1_1 | 158 (2) | O2_3—Ni3_3—O1_3—C10_3 | 143.32 (14) |
O3_1—Ni1'_1—O4_1—Ni1_1 | −13 (2) | O7_3—Ni3_3—O1_3—C1_3 | −64.11 (17) |
O6_1—Ni1_1—O5_1—C8_1 | 95.10 (17) | O6_3—Ni3_3—O1_3—C1_3 | 112.35 (16) |
O7_1—Ni1_1—O5_1—C8_1 | −101.00 (17) | O3_3—Ni3_3—O1_3—C1_3 | 35.8 (3) |
O3_1—Ni1_1—O5_1—C8_1 | 9.8 (5) | O5_3—Ni3_3—O1_3—C1_3 | −154.14 (14) |
O4_1—Ni1_1—O5_1—C8_1 | −7.01 (18) | O4_3—Ni3_3—O1_3—C1_3 | −153.7 (2) |
O2_1—Ni1_1—O5_1—C8_1 | −174.0 (2) | O2_3—Ni3_3—O1_3—C1_3 | 17.13 (15) |
O1_1—Ni1_1—O5_1—C8_1 | 177.72 (15) | O7_3—Ni3_3—O1_3—Ni3'_3 | −82.5 (18) |
O6_1—Ni1_1—O5_1—C9_1 | −82.90 (19) | O6_3—Ni3_3—O1_3—Ni3'_3 | 94.0 (18) |
O7_1—Ni1_1—O5_1—C9_1 | 80.99 (19) | O3_3—Ni3_3—O1_3—Ni3'_3 | 17.4 (15) |
O3_1—Ni1_1—O5_1—C9_1 | −168.2 (3) | O5_3—Ni3_3—O1_3—Ni3'_3 | −172.5 (18) |
O4_1—Ni1_1—O5_1—C9_1 | 174.98 (16) | O4_3—Ni3_3—O1_3—Ni3'_3 | −172 (2) |
O2_1—Ni1_1—O5_1—C9_1 | 8.0 (3) | O2_3—Ni3_3—O1_3—Ni3'_3 | −1.2 (17) |
O1_1—Ni1_1—O5_1—C9_1 | −0.29 (18) | O7_3—Ni3'_3—O2_3—C3_3 | −113.97 (15) |
O6_1—Ni1_1—O5_1—Ni1'_1 | −85.4 (7) | O6_3—Ni3'_3—O2_3—C3_3 | 60.01 (18) |
O7_1—Ni1_1—O5_1—Ni1'_1 | 78.5 (6) | O1_3—Ni3'_3—O2_3—C3_3 | 149.30 (14) |
O3_1—Ni1_1—O5_1—Ni1'_1 | −170.7 (10) | O5_3—Ni3'_3—O2_3—C3_3 | 166.5 (2) |
O4_1—Ni1_1—O5_1—Ni1'_1 | 172.5 (7) | O3_3—Ni3'_3—O2_3—C3_3 | −19.61 (15) |
O2_1—Ni1_1—O5_1—Ni1'_1 | 5.5 (5) | O4_3—Ni3'_3—O2_3—C3_3 | −38.7 (2) |
O1_1—Ni1_1—O5_1—Ni1'_1 | −2.8 (6) | O7_3—Ni3'_3—O2_3—C2_3 | 112.82 (15) |
O7_1—Ni1'_1—O5_1—C8_1 | −89.01 (19) | O6_3—Ni3'_3—O2_3—C2_3 | −73.20 (17) |
O6_1—Ni1'_1—O5_1—C8_1 | 83.65 (19) | O1_3—Ni3'_3—O2_3—C2_3 | 16.09 (15) |
O2_1—Ni1'_1—O5_1—C8_1 | −169.5 (2) | O5_3—Ni3'_3—O2_3—C2_3 | 33.3 (3) |
O1_1—Ni1'_1—O5_1—C8_1 | 177.42 (17) | O3_3—Ni3'_3—O2_3—C2_3 | −152.82 (14) |
O3_1—Ni1'_1—O5_1—C8_1 | 5.7 (2) | O4_3—Ni3'_3—O2_3—C2_3 | −171.92 (17) |
O4_1—Ni1'_1—O5_1—C8_1 | −6.11 (16) | O7_3—Ni3'_3—O2_3—Ni3_3 | −82.5 (10) |
O7_1—Ni1'_1—O5_1—C9_1 | 92.63 (16) | O6_3—Ni3'_3—O2_3—Ni3_3 | 91.5 (10) |
O6_1—Ni1'_1—O5_1—C9_1 | −94.70 (16) | O1_3—Ni3'_3—O2_3—Ni3_3 | −179.2 (11) |
O2_1—Ni1'_1—O5_1—C9_1 | 12.1 (3) | O5_3—Ni3'_3—O2_3—Ni3_3 | −162.0 (12) |
O1_1—Ni1'_1—O5_1—C9_1 | −0.93 (13) | O3_3—Ni3'_3—O2_3—Ni3_3 | 11.9 (10) |
O3_1—Ni1'_1—O5_1—C9_1 | −172.63 (14) | O4_3—Ni3'_3—O2_3—Ni3_3 | −7.2 (9) |
O4_1—Ni1'_1—O5_1—C9_1 | 175.54 (14) | O7_3—Ni3_3—O2_3—C3_3 | −120.28 (15) |
O7_1—Ni1'_1—O5_1—Ni1_1 | −89.6 (7) | O6_3—Ni3_3—O2_3—C3_3 | 71.42 (17) |
O6_1—Ni1'_1—O5_1—Ni1_1 | 83.1 (7) | O3_3—Ni3_3—O2_3—C3_3 | −16.53 (16) |
O2_1—Ni1'_1—O5_1—Ni1_1 | −170.0 (8) | O5_3—Ni3_3—O2_3—C3_3 | 162.0 (2) |
O1_1—Ni1'_1—O5_1—Ni1_1 | 176.9 (7) | O4_3—Ni3_3—O2_3—C3_3 | −41.0 (4) |
O3_1—Ni1'_1—O5_1—Ni1_1 | 5.2 (6) | O1_3—Ni3_3—O2_3—C3_3 | 150.95 (14) |
O4_1—Ni1'_1—O5_1—Ni1_1 | −6.7 (6) | O7_3—Ni3_3—O2_3—C2_3 | 105.86 (17) |
O7_1—Ni1_1—O6_1—Ni1'_1 | 10.6 (2) | O6_3—Ni3_3—O2_3—C2_3 | −62.4 (2) |
O3_1—Ni1_1—O6_1—Ni1'_1 | −120.3 (7) | O3_3—Ni3_3—O2_3—C2_3 | −150.39 (16) |
O4_1—Ni1_1—O6_1—Ni1'_1 | 159.7 (7) | O5_3—Ni3_3—O2_3—C2_3 | 28.1 (3) |
O5_1—Ni1_1—O6_1—Ni1'_1 | 87.0 (6) | O4_3—Ni3_3—O2_3—C2_3 | −174.9 (3) |
O2_1—Ni1_1—O6_1—Ni1'_1 | −46.4 (6) | O1_3—Ni3_3—O2_3—C2_3 | 17.09 (17) |
O1_1—Ni1_1—O6_1—Ni1'_1 | 19.9 (6) | O7_3—Ni3_3—O2_3—Ni3'_3 | 89.5 (10) |
O2_1—Ni1'_1—O6_1—Ni1_1 | 123.9 (7) | O6_3—Ni3_3—O2_3—Ni3'_3 | −78.8 (10) |
O1_1—Ni1'_1—O6_1—Ni1_1 | −156.5 (7) | O3_3—Ni3_3—O2_3—Ni3'_3 | −166.8 (11) |
O5_1—Ni1'_1—O6_1—Ni1_1 | −82.4 (6) | O5_3—Ni3_3—O2_3—Ni3'_3 | 11.8 (8) |
O3_1—Ni1'_1—O6_1—Ni1_1 | 51.1 (6) | O4_3—Ni3_3—O2_3—Ni3'_3 | 168.8 (13) |
O4_1—Ni1'_1—O6_1—Ni1_1 | −16.7 (6) | O1_3—Ni3_3—O2_3—Ni3'_3 | 0.7 (10) |
O2_1—Ni1'_1—O7_1—Ni1_1 | −124.6 (7) | O7_3—Ni3_3—O3_3—C4_3 | 59.45 (18) |
O1_1—Ni1'_1—O7_1—Ni1_1 | 156.3 (7) | O6_3—Ni3_3—O3_3—C4_3 | −108.69 (16) |
O5_1—Ni1'_1—O7_1—Ni1_1 | 82.0 (7) | O5_3—Ni3_3—O3_3—C4_3 | 165.3 (3) |
O3_1—Ni1'_1—O7_1—Ni1_1 | −50.5 (6) | O4_3—Ni3_3—O3_3—C4_3 | 151.22 (14) |
O4_1—Ni1'_1—O7_1—Ni1_1 | 16.5 (6) | O2_3—Ni3_3—O3_3—C4_3 | −16.98 (17) |
O6_1—Ni1_1—O7_1—Ni1'_1 | −10.8 (2) | O1_3—Ni3_3—O3_3—C4_3 | −34.9 (3) |
O3_1—Ni1_1—O7_1—Ni1'_1 | 119.0 (7) | O7_3—Ni3_3—O3_3—C5_3 | −74.19 (18) |
O4_1—Ni1_1—O7_1—Ni1'_1 | −160.4 (7) | O6_3—Ni3_3—O3_3—C5_3 | 117.67 (15) |
O5_1—Ni1_1—O7_1—Ni1'_1 | −86.9 (6) | O5_3—Ni3_3—O3_3—C5_3 | 31.7 (5) |
O2_1—Ni1_1—O7_1—Ni1'_1 | 47.9 (6) | O4_3—Ni3_3—O3_3—C5_3 | 17.58 (17) |
O1_1—Ni1_1—O7_1—Ni1'_1 | −20.1 (6) | O2_3—Ni3_3—O3_3—C5_3 | −150.62 (15) |
C10_1—O1_1—C1_1—C2_1 | 169.02 (16) | O1_3—Ni3_3—O3_3—C5_3 | −168.5 (2) |
Ni1'_1—O1_1—C1_1—C2_1 | 44.72 (18) | O7_3—Ni3_3—O3_3—Ni3'_3 | 86.7 (9) |
Ni1_1—O1_1—C1_1—C2_1 | 45.8 (2) | O6_3—Ni3_3—O3_3—Ni3'_3 | −81.5 (9) |
C3_1—O2_1—C2_1—C1_1 | 178.00 (17) | O5_3—Ni3_3—O3_3—Ni3'_3 | −167.5 (13) |
Ni1'_1—O2_1—C2_1—C1_1 | 44.09 (19) | O4_3—Ni3_3—O3_3—Ni3'_3 | 178.4 (10) |
Ni1_1—O2_1—C2_1—C1_1 | 46.9 (2) | O2_3—Ni3_3—O3_3—Ni3'_3 | 10.2 (8) |
O1_1—C1_1—C2_1—O2_1 | −58.5 (2) | O1_3—Ni3_3—O3_3—Ni3'_3 | −7.6 (7) |
C2_1—O2_1—C3_1—C4_1 | 177.87 (17) | O7_3—Ni3'_3—O3_3—C4_3 | 72.65 (15) |
Ni1'_1—O2_1—C3_1—C4_1 | −50.4 (2) | O6_3—Ni3'_3—O3_3—C4_3 | −116.39 (14) |
Ni1_1—O2_1—C3_1—C4_1 | −45.9 (2) | O2_3—Ni3'_3—O3_3—C4_3 | −13.86 (14) |
C5_1—O3_1—C4_1—C3_1 | −173.63 (17) | O1_3—Ni3'_3—O3_3—C4_3 | −38.2 (3) |
Ni1_1—O3_1—C4_1—C3_1 | −44.0 (2) | O5_3—Ni3'_3—O3_3—C4_3 | 162.22 (16) |
Ni1'_1—O3_1—C4_1—C3_1 | −40.38 (19) | O4_3—Ni3'_3—O3_3—C4_3 | 153.15 (13) |
O2_1—C3_1—C4_1—O3_1 | 57.5 (2) | O7_3—Ni3'_3—O3_3—C5_3 | −61.27 (18) |
C4_1—O3_1—C5_1—C6_1 | −176.71 (17) | O6_3—Ni3'_3—O3_3—C5_3 | 109.69 (16) |
Ni1_1—O3_1—C5_1—C6_1 | 49.1 (2) | O2_3—Ni3'_3—O3_3—C5_3 | −147.78 (16) |
Ni1'_1—O3_1—C5_1—C6_1 | 53.6 (2) | O1_3—Ni3'_3—O3_3—C5_3 | −172.2 (2) |
C7_1—O4_1—C6_1—C5_1 | 164.24 (17) | O5_3—Ni3'_3—O3_3—C5_3 | 28.3 (2) |
Ni1_1—O4_1—C6_1—C5_1 | 42.3 (2) | O4_3—Ni3'_3—O3_3—C5_3 | 19.23 (15) |
Ni1'_1—O4_1—C6_1—C5_1 | 42.2 (2) | O7_3—Ni3'_3—O3_3—Ni3_3 | −81.9 (9) |
O3_1—C5_1—C6_1—O4_1 | −61.0 (2) | O6_3—Ni3'_3—O3_3—Ni3_3 | 89.1 (9) |
C6_1—O4_1—C7_1—C8_1 | −177.24 (17) | O2_3—Ni3'_3—O3_3—Ni3_3 | −168.4 (10) |
Ni1_1—O4_1—C7_1—C8_1 | −56.0 (2) | O1_3—Ni3'_3—O3_3—Ni3_3 | 167.2 (11) |
Ni1'_1—O4_1—C7_1—C8_1 | −53.09 (18) | O5_3—Ni3'_3—O3_3—Ni3_3 | 7.7 (8) |
C9_1—O5_1—C8_1—C7_1 | 158.38 (17) | O4_3—Ni3'_3—O3_3—Ni3_3 | −1.4 (9) |
Ni1_1—O5_1—C8_1—C7_1 | −19.9 (2) | O7_3—Ni3_3—O4_3—C7_3 | −120.50 (16) |
Ni1'_1—O5_1—C8_1—C7_1 | −20.0 (2) | O6_3—Ni3_3—O4_3—C7_3 | 53.29 (19) |
O4_1—C7_1—C8_1—O5_1 | 47.9 (2) | O3_3—Ni3_3—O4_3—C7_3 | 139.75 (15) |
C8_1—O5_1—C9_1—C10_1 | 154.09 (17) | O5_3—Ni3_3—O4_3—C7_3 | −33.54 (16) |
Ni1_1—O5_1—C9_1—C10_1 | −27.9 (2) | O2_3—Ni3_3—O4_3—C7_3 | 163.7 (3) |
Ni1'_1—O5_1—C9_1—C10_1 | −27.3 (2) | O1_3—Ni3_3—O4_3—C7_3 | −34.0 (3) |
C1_1—O1_1—C10_1—C9_1 | −177.96 (16) | O7_3—Ni3_3—O4_3—C6_3 | 115.00 (17) |
Ni1'_1—O1_1—C10_1—C9_1 | −54.97 (18) | O6_3—Ni3_3—O4_3—C6_3 | −71.22 (19) |
Ni1_1—O1_1—C10_1—C9_1 | −52.40 (19) | O3_3—Ni3_3—O4_3—C6_3 | 15.24 (17) |
O5_1—C9_1—C10_1—O1_1 | 51.6 (2) | O5_3—Ni3_3—O4_3—C6_3 | −158.05 (15) |
O7_2—Ni2'_2—O1_2—C10_2 | 57.86 (17) | O2_3—Ni3_3—O4_3—C6_3 | 39.2 (4) |
O6_2—Ni2'_2—O1_2—C10_2 | −114.92 (15) | O1_3—Ni3_3—O4_3—C6_3 | −158.5 (2) |
O2_2—Ni2'_2—O1_2—C10_2 | 142.90 (14) | O7_3—Ni3_3—O4_3—Ni3'_3 | −75 (3) |
O5_2—Ni2'_2—O1_2—C10_2 | −28.66 (15) | O6_3—Ni3_3—O4_3—Ni3'_3 | 99 (3) |
O3_2—Ni2'_2—O1_2—C10_2 | 164.6 (2) | O3_3—Ni3_3—O4_3—Ni3'_3 | −175 (3) |
O4_2—Ni2'_2—O1_2—C10_2 | −27.9 (2) | O5_3—Ni3_3—O4_3—Ni3'_3 | 12 (3) |
O7_2—Ni2'_2—O1_2—C1_2 | −67.04 (16) | O2_3—Ni3_3—O4_3—Ni3'_3 | −151 (3) |
O6_2—Ni2'_2—O1_2—C1_2 | 120.18 (14) | O1_3—Ni3_3—O4_3—Ni3'_3 | 11 (3) |
O2_2—Ni2'_2—O1_2—C1_2 | 18.00 (14) | O7_3—Ni3'_3—O4_3—C7_3 | −122.81 (14) |
O5_2—Ni2'_2—O1_2—C1_2 | −153.56 (13) | O6_3—Ni3'_3—O4_3—C7_3 | 57.10 (14) |
O3_2—Ni2'_2—O1_2—C1_2 | 39.7 (3) | O2_3—Ni3'_3—O4_3—C7_3 | 160.24 (18) |
O4_2—Ni2'_2—O1_2—C1_2 | −152.79 (18) | O1_3—Ni3'_3—O4_3—C7_3 | −31.9 (2) |
O7_2—Ni2'_2—O1_2—Ni2_2 | 92 (2) | O5_3—Ni3'_3—O4_3—C7_3 | −32.51 (13) |
O6_2—Ni2'_2—O1_2—Ni2_2 | −80 (2) | O3_3—Ni3'_3—O4_3—C7_3 | 140.17 (14) |
O2_2—Ni2'_2—O1_2—Ni2_2 | 177 (2) | O7_3—Ni3'_3—O4_3—C6_3 | 112.24 (15) |
O5_2—Ni2'_2—O1_2—Ni2_2 | 5.8 (19) | O6_3—Ni3'_3—O4_3—C6_3 | −67.86 (16) |
O3_2—Ni2'_2—O1_2—Ni2_2 | −161 (2) | O2_3—Ni3'_3—O4_3—C6_3 | 35.3 (2) |
O4_2—Ni2'_2—O1_2—Ni2_2 | 6.6 (18) | O1_3—Ni3'_3—O4_3—C6_3 | −156.82 (18) |
O6_2—Ni2_2—O1_2—C10_2 | −118.53 (15) | O5_3—Ni3'_3—O4_3—C6_3 | −157.46 (15) |
O7_2—Ni2_2—O1_2—C10_2 | 63.14 (16) | O3_3—Ni3'_3—O4_3—C6_3 | 15.22 (14) |
O3_2—Ni2_2—O1_2—C10_2 | 161.6 (2) | O7_3—Ni3'_3—O4_3—Ni3_3 | 102 (3) |
O4_2—Ni2_2—O1_2—C10_2 | −25.7 (3) | O6_3—Ni3'_3—O4_3—Ni3_3 | −78 (3) |
O5_2—Ni2_2—O1_2—C10_2 | −27.56 (15) | O2_3—Ni3'_3—O4_3—Ni3_3 | 25 (3) |
O2_2—Ni2_2—O1_2—C10_2 | 143.81 (14) | O1_3—Ni3'_3—O4_3—Ni3_3 | −167 (3) |
O6_2—Ni2_2—O1_2—C1_2 | 116.32 (15) | O5_3—Ni3'_3—O4_3—Ni3_3 | −168 (3) |
O7_2—Ni2_2—O1_2—C1_2 | −62.01 (16) | O3_3—Ni3'_3—O4_3—Ni3_3 | 5 (3) |
O3_2—Ni2_2—O1_2—C1_2 | 36.5 (3) | O7_3—Ni3_3—O5_3—C8_3 | 100.24 (17) |
O4_2—Ni2_2—O1_2—C1_2 | −150.8 (2) | O6_3—Ni3_3—O5_3—C8_3 | −94.17 (17) |
O5_2—Ni2_2—O1_2—C1_2 | −152.71 (14) | O3_3—Ni3_3—O5_3—C8_3 | −8.5 (5) |
O2_2—Ni2_2—O1_2—C1_2 | 18.66 (14) | O4_3—Ni3_3—O5_3—C8_3 | 5.93 (18) |
O6_2—Ni2_2—O1_2—Ni2'_2 | 95 (2) | O2_3—Ni3_3—O5_3—C8_3 | 174.6 (2) |
O7_2—Ni2_2—O1_2—Ni2'_2 | −83 (2) | O1_3—Ni3_3—O5_3—C8_3 | −174.37 (15) |
O3_2—Ni2_2—O1_2—Ni2'_2 | 15.3 (18) | O7_3—Ni3_3—O5_3—C9_3 | −87.58 (19) |
O4_2—Ni2_2—O1_2—Ni2'_2 | −172 (2) | O6_3—Ni3_3—O5_3—C9_3 | 78.0 (2) |
O5_2—Ni2_2—O1_2—Ni2'_2 | −174 (2) | O3_3—Ni3_3—O5_3—C9_3 | 163.7 (3) |
O2_2—Ni2_2—O1_2—Ni2'_2 | −2.5 (19) | O4_3—Ni3_3—O5_3—C9_3 | 178.11 (16) |
O7_2—Ni2'_2—O2_2—C2_2 | 110.70 (15) | O2_3—Ni3_3—O5_3—C9_3 | −13.3 (3) |
O6_2—Ni2'_2—O2_2—C2_2 | −77.03 (17) | O1_3—Ni3_3—O5_3—C9_3 | −2.18 (18) |
O1_2—Ni2'_2—O2_2—C2_2 | 14.52 (15) | O7_3—Ni3_3—O5_3—Ni3'_3 | −82.4 (8) |
O5_2—Ni2'_2—O2_2—C2_2 | 33.0 (3) | O6_3—Ni3_3—O5_3—Ni3'_3 | 83.1 (8) |
O3_2—Ni2'_2—O2_2—C2_2 | −154.60 (14) | O3_3—Ni3_3—O5_3—Ni3'_3 | 168.8 (11) |
O4_2—Ni2'_2—O2_2—C2_2 | −174.21 (17) | O4_3—Ni3_3—O5_3—Ni3'_3 | −176.8 (8) |
O7_2—Ni2'_2—O2_2—C3_2 | −114.68 (15) | O2_3—Ni3_3—O5_3—Ni3'_3 | −8.1 (6) |
O6_2—Ni2'_2—O2_2—C3_2 | 57.58 (18) | O1_3—Ni3_3—O5_3—Ni3'_3 | 3.0 (7) |
O1_2—Ni2'_2—O2_2—C3_2 | 149.13 (15) | O7_3—Ni3'_3—O5_3—C8_3 | 89.09 (19) |
O5_2—Ni2'_2—O2_2—C3_2 | 167.6 (3) | O6_3—Ni3'_3—O5_3—C8_3 | −82.07 (19) |
O3_2—Ni2'_2—O2_2—C3_2 | −19.99 (15) | O2_3—Ni3'_3—O5_3—C8_3 | 168.7 (2) |
O4_2—Ni2'_2—O2_2—C3_2 | −39.6 (2) | O1_3—Ni3'_3—O5_3—C8_3 | −173.65 (17) |
O7_2—Ni2'_2—O2_2—Ni2_2 | −82.5 (9) | O3_3—Ni3'_3—O5_3—C8_3 | −3.3 (3) |
O6_2—Ni2'_2—O2_2—Ni2_2 | 89.8 (9) | O4_3—Ni3'_3—O5_3—C8_3 | 5.92 (17) |
O1_2—Ni2'_2—O2_2—Ni2_2 | −178.7 (10) | O7_3—Ni3'_3—O5_3—C9_3 | −98.51 (16) |
O5_2—Ni2'_2—O2_2—Ni2_2 | −160.2 (12) | O6_3—Ni3'_3—O5_3—C9_3 | 90.34 (16) |
O3_2—Ni2'_2—O2_2—Ni2_2 | 12.2 (9) | O2_3—Ni3'_3—O5_3—C9_3 | −18.9 (3) |
O4_2—Ni2'_2—O2_2—Ni2_2 | −7.4 (8) | O1_3—Ni3'_3—O5_3—C9_3 | −1.24 (15) |
O6_2—Ni2_2—O2_2—C2_2 | −65.17 (19) | O3_3—Ni3'_3—O5_3—C9_3 | 169.14 (15) |
O7_2—Ni2_2—O2_2—C2_2 | 103.15 (16) | O4_3—Ni3'_3—O5_3—C9_3 | 178.32 (15) |
O3_2—Ni2_2—O2_2—C2_2 | −152.21 (15) | O7_3—Ni3'_3—O5_3—Ni3_3 | 86.1 (8) |
O4_2—Ni2_2—O2_2—C2_2 | −177.5 (3) | O6_3—Ni3'_3—O5_3—Ni3_3 | −85.1 (8) |
O5_2—Ni2_2—O2_2—C2_2 | 26.5 (3) | O2_3—Ni3'_3—O5_3—Ni3_3 | 165.7 (10) |
O1_2—Ni2_2—O2_2—C2_2 | 15.35 (16) | O1_3—Ni3'_3—O5_3—Ni3_3 | −176.7 (8) |
O6_2—Ni2_2—O2_2—C3_2 | 70.47 (17) | O3_3—Ni3'_3—O5_3—Ni3_3 | −6.3 (6) |
O7_2—Ni2_2—O2_2—C3_2 | −121.21 (15) | O4_3—Ni3'_3—O5_3—Ni3_3 | 2.9 (7) |
O3_2—Ni2_2—O2_2—C3_2 | −16.56 (15) | O2_3—Ni3'_3—O6_3—Ni3_3 | −127.8 (8) |
O4_2—Ni2_2—O2_2—C3_2 | −41.9 (4) | O1_3—Ni3'_3—O6_3—Ni3_3 | 152.6 (8) |
O5_2—Ni2_2—O2_2—C3_2 | 162.1 (2) | O5_3—Ni3'_3—O6_3—Ni3_3 | 79.1 (8) |
O1_2—Ni2_2—O2_2—C3_2 | 151.00 (14) | O3_3—Ni3'_3—O6_3—Ni3_3 | −54.1 (8) |
O6_2—Ni2_2—O2_2—Ni2'_2 | −79.4 (9) | O4_3—Ni3'_3—O6_3—Ni3_3 | 13.4 (7) |
O7_2—Ni2_2—O2_2—Ni2'_2 | 89.0 (9) | O7_3—Ni3_3—O6_3—Ni3'_3 | −9.3 (3) |
O3_2—Ni2_2—O2_2—Ni2'_2 | −166.4 (10) | O3_3—Ni3_3—O6_3—Ni3'_3 | 117.3 (8) |
O4_2—Ni2_2—O2_2—Ni2'_2 | 168.3 (12) | O5_3—Ni3_3—O6_3—Ni3'_3 | −90.1 (8) |
O5_2—Ni2_2—O2_2—Ni2'_2 | 12.3 (7) | O4_3—Ni3_3—O6_3—Ni3'_3 | −163.9 (9) |
O1_2—Ni2_2—O2_2—Ni2'_2 | 1.2 (9) | O2_3—Ni3_3—O6_3—Ni3'_3 | 43.2 (7) |
O6_2—Ni2_2—O3_2—C4_2 | −110.94 (16) | O1_3—Ni3_3—O6_3—Ni3'_3 | −23.4 (7) |
O7_2—Ni2_2—O3_2—C4_2 | 58.87 (18) | O2_3—Ni3'_3—O7_3—Ni3_3 | 128.5 (8) |
O4_2—Ni2_2—O3_2—C4_2 | 151.39 (14) | O1_3—Ni3'_3—O7_3—Ni3_3 | −152.3 (9) |
O5_2—Ni2_2—O3_2—C4_2 | 166.0 (3) | O5_3—Ni3'_3—O7_3—Ni3_3 | −79.2 (8) |
O2_2—Ni2_2—O3_2—C4_2 | −16.02 (16) | O3_3—Ni3'_3—O7_3—Ni3_3 | 53.2 (8) |
O1_2—Ni2_2—O3_2—C4_2 | −33.2 (3) | O4_3—Ni3'_3—O7_3—Ni3_3 | −13.4 (8) |
O6_2—Ni2_2—O3_2—C5_2 | 117.69 (15) | O6_3—Ni3_3—O7_3—Ni3'_3 | 9.3 (3) |
O7_2—Ni2_2—O3_2—C5_2 | −72.50 (16) | O3_3—Ni3_3—O7_3—Ni3'_3 | −116.1 (8) |
O4_2—Ni2_2—O3_2—C5_2 | 20.02 (16) | O5_3—Ni3_3—O7_3—Ni3'_3 | 90.3 (8) |
O5_2—Ni2_2—O3_2—C5_2 | 34.7 (4) | O4_3—Ni3_3—O7_3—Ni3'_3 | 164.2 (9) |
O2_2—Ni2_2—O3_2—C5_2 | −147.39 (14) | O2_3—Ni3_3—O7_3—Ni3'_3 | −44.3 (7) |
O1_2—Ni2_2—O3_2—C5_2 | −164.5 (2) | O1_3—Ni3_3—O7_3—Ni3'_3 | 23.3 (7) |
O6_2—Ni2_2—O3_2—Ni2'_2 | −83.6 (9) | C10_3—O1_3—C1_3—C2_3 | −169.24 (17) |
O7_2—Ni2_2—O3_2—Ni2'_2 | 86.2 (9) | Ni3'_3—O1_3—C1_3—C2_3 | −44.3 (2) |
O4_2—Ni2_2—O3_2—Ni2'_2 | 178.7 (10) | Ni3_3—O1_3—C1_3—C2_3 | −45.7 (2) |
O5_2—Ni2_2—O3_2—Ni2'_2 | −166.6 (12) | C3_3—O2_3—C2_3—C1_3 | −178.69 (17) |
O2_2—Ni2_2—O3_2—Ni2'_2 | 11.3 (8) | Ni3'_3—O2_3—C2_3—C1_3 | −44.4 (2) |
O1_2—Ni2_2—O3_2—Ni2'_2 | −5.8 (7) | Ni3_3—O2_3—C2_3—C1_3 | −46.8 (2) |
O7_2—Ni2'_2—O3_2—C4_2 | 72.21 (16) | O1_3—C1_3—C2_3—O2_3 | 58.3 (2) |
O6_2—Ni2'_2—O3_2—C4_2 | −118.56 (14) | C2_3—O2_3—C3_3—C4_3 | −179.55 (17) |
O2_2—Ni2'_2—O3_2—C4_2 | −12.73 (14) | Ni3'_3—O2_3—C3_3—C4_3 | 48.1 (2) |
O1_2—Ni2'_2—O3_2—C4_2 | −35.0 (3) | Ni3_3—O2_3—C3_3—C4_3 | 43.6 (2) |
O5_2—Ni2'_2—O3_2—C4_2 | 162.62 (16) | C5_3—O3_3—C4_3—C3_3 | 178.31 (17) |
O4_2—Ni2'_2—O3_2—C4_2 | 153.40 (13) | Ni3_3—O3_3—C4_3—C3_3 | 46.2 (2) |
O7_2—Ni2'_2—O3_2—C5_2 | −59.59 (17) | Ni3'_3—O3_3—C4_3—C3_3 | 41.75 (18) |
O6_2—Ni2'_2—O3_2—C5_2 | 109.64 (16) | O2_3—C3_3—C4_3—O3_3 | −57.3 (2) |
O2_2—Ni2'_2—O3_2—C5_2 | −144.53 (15) | C4_3—O3_3—C5_3—C6_3 | 178.55 (17) |
O1_2—Ni2'_2—O3_2—C5_2 | −166.8 (2) | Ni3_3—O3_3—C5_3—C6_3 | −46.3 (2) |
O5_2—Ni2'_2—O3_2—C5_2 | 30.8 (2) | Ni3'_3—O3_3—C5_3—C6_3 | −49.8 (2) |
O4_2—Ni2'_2—O3_2—C5_2 | 21.59 (14) | C7_3—O4_3—C6_3—C5_3 | −165.27 (18) |
O7_2—Ni2'_2—O3_2—Ni2_2 | −82.3 (9) | Ni3_3—O4_3—C6_3—C5_3 | −43.6 (2) |
O6_2—Ni2'_2—O3_2—Ni2_2 | 86.9 (9) | Ni3'_3—O4_3—C6_3—C5_3 | −44.1 (2) |
O2_2—Ni2'_2—O3_2—Ni2_2 | −167.3 (9) | O3_3—C5_3—C6_3—O4_3 | 59.6 (2) |
O1_2—Ni2'_2—O3_2—Ni2_2 | 170.5 (11) | C6_3—O4_3—C7_3—C8_3 | 176.15 (17) |
O5_2—Ni2'_2—O3_2—Ni2_2 | 8.1 (8) | Ni3_3—O4_3—C7_3—C8_3 | 55.1 (2) |
O4_2—Ni2'_2—O3_2—Ni2_2 | −1.1 (8) | Ni3'_3—O4_3—C7_3—C8_3 | 53.21 (19) |
O6_2—Ni2_2—O4_2—C7_2 | 51.54 (18) | C9_3—O5_3—C8_3—C7_3 | −152.15 (18) |
O7_2—Ni2_2—O4_2—C7_2 | −121.58 (16) | Ni3_3—O5_3—C8_3—C7_3 | 20.9 (2) |
O3_2—Ni2_2—O4_2—C7_2 | 138.63 (14) | Ni3'_3—O5_3—C8_3—C7_3 | 20.3 (3) |
O5_2—Ni2_2—O4_2—C7_2 | −34.58 (15) | O4_3—C7_3—C8_3—O5_3 | −48.5 (2) |
O2_2—Ni2_2—O4_2—C7_2 | 163.1 (3) | C8_3—O5_3—C9_3—C10_3 | −157.43 (17) |
O1_2—Ni2_2—O4_2—C7_2 | −36.4 (3) | Ni3_3—O5_3—C9_3—C10_3 | 30.3 (2) |
O6_2—Ni2_2—O4_2—C6_2 | −74.06 (18) | Ni3'_3—O5_3—C9_3—C10_3 | 29.2 (2) |
O7_2—Ni2_2—O4_2—C6_2 | 112.82 (16) | C1_3—O1_3—C10_3—C9_3 | 176.07 (17) |
O3_2—Ni2_2—O4_2—C6_2 | 13.04 (16) | Ni3'_3—O1_3—C10_3—C9_3 | 53.45 (19) |
O5_2—Ni2_2—O4_2—C6_2 | −160.17 (14) | Ni3_3—O1_3—C10_3—C9_3 | 50.71 (19) |
O2_2—Ni2_2—O4_2—C6_2 | 37.5 (4) | O5_3—C9_3—C10_3—O1_3 | −51.7 (2) |
O1_2—Ni2_2—O4_2—C6_2 | −162.0 (2) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O6_1—H6W1_1···O9_8i | 0.83 (1) | 1.90 (1) | 2.715 (2) | 165 (2) |
O6_1—H6W2_1···O9_7 | 0.81 (1) | 2.22 (2) | 2.958 (2) | 151 (2) |
O6_1—H6W2_1···O8_7 | 0.81 (1) | 2.27 (1) | 3.004 (2) | 150 (2) |
O7_1—H7W1_1···O9_6ii | 0.83 (1) | 1.97 (1) | 2.795 (2) | 170 (2) |
O7_1—H7W1_1···O10_6ii | 0.83 (1) | 2.45 (2) | 3.067 (2) | 132 (2) |
O7_1—H7W2_1···O8_4 | 0.84 (1) | 1.88 (1) | 2.725 (2) | 175 (2) |
O6_2—H6W1_2···O9_4iii | 0.83 (1) | 1.93 (1) | 2.726 (2) | 162 (2) |
O6_2—H6W2_2···O8_5 | 0.83 (1) | 1.93 (1) | 2.754 (2) | 175 (2) |
O6_2—H6W2_2···O9_5 | 0.83 (1) | 2.57 (2) | 3.161 (2) | 129 (2) |
O7_2—H7W1_2···O8_8 | 0.84 (1) | 1.90 (1) | 2.729 (2) | 171 (2) |
O7_2—H7W2_2···O9_9i | 0.83 (1) | 1.89 (1) | 2.715 (2) | 171 (2) |
O7_2—H7W2_2···O10_9i | 0.83 (1) | 2.64 (2) | 3.276 (2) | 135 (2) |
O6_3—H6W1_3···O9_5iii | 0.83 (1) | 1.87 (1) | 2.695 (2) | 171 (2) |
O6_3—H6W2_3···O9_6 | 0.83 (1) | 2.01 (1) | 2.822 (2) | 165 (2) |
O6_3—H6W2_3···O8_6 | 0.83 (1) | 2.47 (2) | 3.093 (2) | 133 (2) |
O7_3—H7W1_3···O9_7iv | 0.83 (1) | 1.92 (1) | 2.739 (2) | 171 (2) |
O7_3—H7W1_3···O10_7iv | 0.83 (1) | 2.57 (2) | 3.200 (2) | 134 (2) |
O7_3—H7W2_3···O8_9 | 0.83 (1) | 1.92 (1) | 2.743 (2) | 172 (2) |
Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) x, −y+3/2, z−1/2; (iii) x, −y+3/2, z+1/2; (iv) x, −y+1/2, z+1/2. |