In [NiCl(C18H15P)2]·C4H8O, the Ni atom is coordinated by three ligands in a distorted trigonal-planar configuration, with a P-Ni-P angle of 111.52 (2)°. In [NiCl(C18H15P)3], there are three independent molecules in the asymmetric unit, with each Ni-Cl bond on a crystallographic threefold rotation axis. Each Ni centre is tetrahedrally bound. The Ni atoms in both compounds have a d9 configuration and a formal oxidation state of NiI. A comparison is made between the form of [NiCl(PPh3)3] presented here and that of a known toluene solvate.
Supporting information
CCDC references: 150756; 150757
For both compounds, data collection: Locally modified CAD4-Version 5 Software (Enraf-Nonius, 1989); cell refinement: SET4 (de Boer & Duisenberg, 1984); data reduction: HELENA (Spek, 1997); program(s) used to solve structure: DIRDIF (Beurksens et al., 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON (Spek, 2000); software used to prepare material for publication: PLATON.
Crystal data top
[NiCl(C18H15P)2]·C4H8O | F(000) = 1444 |
Mr = 690.80 | Dx = 1.341 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 16.4393 (16) Å | Cell parameters from 25 reflections |
b = 11.2773 (12) Å | θ = 11.6–12.2° |
c = 18.463 (2) Å | µ = 0.77 mm−1 |
β = 90.140 (9)° | T = 150 K |
V = 3422.9 (6) Å3 | Plate, yellow |
Z = 4 | 0.55 × 0.55 × 0.05 mm |
Data collection top
Enraf-Nonius CAD4 diffractometer | 6179 reflections with I > 2σ(I) |
Radiation source: rotating anode | Rint = 0.036 |
Graphite monochromator | θmax = 27.5°, θmin = 2.1° |
w/2θ scans | h = −21→21 |
Absorption correction: ψ scan (North et al., 1968) | k = 0→14 |
Tmin = 0.664, Tmax = 0.953 | l = −23→23 |
16135 measured reflections | 3 standard reflections every 60 min |
7820 independent reflections | intensity decay: <1% |
Refinement top
Refinement on F2 | Primary atom site location: heavy-atom method |
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) = 0.096 | H-atom parameters constrained |
S = 1.02 | w = 1/[σ2(Fo2) + (0.0469P)2 + 2.2443P] where P = (Fo2 + 2Fc2)/3 |
7820 reflections | (Δ/σ)max = 0.002 |
406 parameters | Δρmax = 0.76 e Å−3 |
0 restraints | Δρmin = −0.60 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 | |
Ni1 | 0.225505 (15) | 1.13339 (2) | 0.293206 (14) | 0.01851 (8) | |
Cl1 | 0.26162 (3) | 1.31406 (5) | 0.27529 (4) | 0.03494 (14) | |
P1 | 0.28337 (3) | 0.98560 (4) | 0.23406 (3) | 0.01775 (11) | |
P2 | 0.13810 (3) | 1.06838 (4) | 0.37414 (3) | 0.01771 (11) | |
C1 | 0.25518 (12) | 0.83349 (17) | 0.25459 (10) | 0.0195 (4) | |
C2 | 0.17864 (12) | 0.79355 (18) | 0.23271 (11) | 0.0222 (4) | |
H2 | 0.1445 | 0.8440 | 0.2048 | 0.027* | |
C3 | 0.15176 (14) | 0.6810 (2) | 0.25124 (12) | 0.0278 (5) | |
H3 | 0.0998 | 0.6544 | 0.2356 | 0.033* | |
C4 | 0.20081 (15) | 0.60731 (19) | 0.29267 (12) | 0.0303 (5) | |
H4 | 0.1823 | 0.5305 | 0.3059 | 0.036* | |
C5 | 0.27695 (15) | 0.6462 (2) | 0.31472 (13) | 0.0309 (5) | |
H5 | 0.3106 | 0.5955 | 0.3429 | 0.037* | |
C6 | 0.30442 (13) | 0.75831 (19) | 0.29599 (11) | 0.0257 (4) | |
H6 | 0.3567 | 0.7841 | 0.3113 | 0.031* | |
C7 | 0.39345 (12) | 0.98653 (18) | 0.24452 (11) | 0.0208 (4) | |
C8 | 0.44365 (13) | 0.9113 (2) | 0.20468 (13) | 0.0318 (5) | |
H8 | 0.4205 | 0.8589 | 0.1700 | 0.038* | |
C9 | 0.52689 (14) | 0.9124 (2) | 0.21537 (14) | 0.0356 (5) | |
H9 | 0.5605 | 0.8602 | 0.1884 | 0.043* | |
C10 | 0.56135 (13) | 0.9887 (2) | 0.26498 (14) | 0.0340 (5) | |
H10 | 0.6186 | 0.9890 | 0.2723 | 0.041* | |
C11 | 0.51255 (15) | 1.0646 (2) | 0.30393 (16) | 0.0412 (6) | |
H11 | 0.5362 | 1.1178 | 0.3379 | 0.049* | |
C12 | 0.42869 (14) | 1.0635 (2) | 0.29366 (14) | 0.0326 (5) | |
H12 | 0.3954 | 1.1162 | 0.3207 | 0.039* | |
C13 | 0.26925 (11) | 0.99691 (18) | 0.13605 (10) | 0.0206 (4) | |
C14 | 0.25847 (15) | 1.1099 (2) | 0.10689 (12) | 0.0301 (5) | |
H14 | 0.2546 | 1.1765 | 0.1382 | 0.036* | |
C15 | 0.25340 (17) | 1.1259 (2) | 0.03243 (13) | 0.0390 (6) | |
H15 | 0.2470 | 1.2034 | 0.0130 | 0.047* | |
C16 | 0.25761 (16) | 1.0290 (2) | −0.01348 (12) | 0.0364 (5) | |
H16 | 0.2540 | 1.0400 | −0.0644 | 0.044* | |
C17 | 0.26703 (15) | 0.9162 (2) | 0.01483 (12) | 0.0309 (5) | |
H17 | 0.2694 | 0.8497 | −0.0167 | 0.037* | |
C18 | 0.27303 (13) | 0.89987 (19) | 0.08928 (12) | 0.0258 (4) | |
H18 | 0.2797 | 0.8223 | 0.1084 | 0.031* | |
C19 | 0.18837 (12) | 1.02742 (18) | 0.45891 (11) | 0.0205 (4) | |
C20 | 0.25755 (13) | 0.9565 (2) | 0.45537 (12) | 0.0295 (5) | |
H20 | 0.2777 | 0.9321 | 0.4095 | 0.035* | |
C21 | 0.29750 (15) | 0.9210 (2) | 0.51819 (13) | 0.0341 (5) | |
H21 | 0.3443 | 0.8717 | 0.5153 | 0.041* | |
C22 | 0.26900 (14) | 0.9574 (2) | 0.58477 (13) | 0.0327 (5) | |
H22 | 0.2961 | 0.9328 | 0.6277 | 0.039* | |
C23 | 0.20122 (14) | 1.0295 (2) | 0.58936 (12) | 0.0315 (5) | |
H23 | 0.1824 | 1.0555 | 0.6353 | 0.038* | |
C24 | 0.16051 (13) | 1.06407 (19) | 0.52632 (11) | 0.0249 (4) | |
H24 | 0.1135 | 1.1129 | 0.5295 | 0.030* | |
C25 | 0.06719 (12) | 1.18677 (18) | 0.39963 (10) | 0.0198 (4) | |
C26 | 0.09788 (13) | 1.30164 (19) | 0.40602 (11) | 0.0247 (4) | |
H26 | 0.1544 | 1.3155 | 0.3997 | 0.030* | |
C27 | 0.04647 (15) | 1.3957 (2) | 0.42158 (12) | 0.0308 (5) | |
H27 | 0.0681 | 1.4734 | 0.4266 | 0.037* | |
C28 | −0.03622 (15) | 1.3770 (2) | 0.42981 (12) | 0.0311 (5) | |
H28 | −0.0715 | 1.4419 | 0.4393 | 0.037* | |
C29 | −0.06708 (13) | 1.2634 (2) | 0.42413 (12) | 0.0290 (5) | |
H29 | −0.1237 | 1.2503 | 0.4301 | 0.035* | |
C30 | −0.01590 (13) | 1.16810 (19) | 0.40972 (11) | 0.0242 (4) | |
H30 | −0.0376 | 1.0902 | 0.4067 | 0.029* | |
C31 | 0.06975 (12) | 0.94524 (17) | 0.35483 (10) | 0.0194 (4) | |
C32 | 0.06165 (13) | 0.84804 (18) | 0.40047 (11) | 0.0237 (4) | |
H32 | 0.0949 | 0.8420 | 0.4424 | 0.028* | |
C33 | 0.00514 (14) | 0.7592 (2) | 0.38526 (12) | 0.0290 (5) | |
H33 | 0.0004 | 0.6927 | 0.4165 | 0.035* | |
C34 | −0.04399 (13) | 0.7681 (2) | 0.32472 (13) | 0.0309 (5) | |
H34 | −0.0834 | 0.7085 | 0.3149 | 0.037* | |
C35 | −0.03583 (14) | 0.8638 (2) | 0.27824 (12) | 0.0296 (5) | |
H35 | −0.0693 | 0.8695 | 0.2364 | 0.035* | |
C36 | 0.02111 (13) | 0.95129 (19) | 0.29283 (11) | 0.0245 (4) | |
H36 | 0.0271 | 1.0160 | 0.2603 | 0.029* | |
O40 | 0.5150 (2) | 0.2653 (3) | −0.0369 (2) | 0.1019 (11) | |
C41 | 0.4547 (5) | 0.3297 (6) | −0.0088 (4) | 0.146 (3) | |
H41A | 0.4018 | 0.3073 | −0.0305 | 0.176* | |
H41B | 0.4640 | 0.4154 | −0.0170 | 0.176* | |
C42 | 0.4564 (4) | 0.3010 (6) | 0.0714 (4) | 0.154 (3) | |
H42A | 0.4015 | 0.3064 | 0.0931 | 0.185* | |
H42B | 0.4941 | 0.3538 | 0.0981 | 0.185* | |
C43 | 0.4872 (4) | 0.1736 (6) | 0.0701 (3) | 0.118 (2) | |
H43A | 0.5378 | 0.1643 | 0.0987 | 0.142* | |
H43B | 0.4457 | 0.1172 | 0.0880 | 0.142* | |
C44 | 0.5025 (3) | 0.1585 (4) | −0.0106 (3) | 0.0874 (13) | |
H44A | 0.5507 | 0.1076 | −0.0188 | 0.105* | |
H44B | 0.4549 | 0.1213 | −0.0344 | 0.105* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.02001 (13) | 0.01546 (13) | 0.02009 (13) | −0.00005 (10) | 0.00268 (9) | −0.00049 (10) |
Cl1 | 0.0318 (3) | 0.0177 (2) | 0.0554 (4) | −0.0031 (2) | 0.0088 (2) | 0.0018 (2) |
P1 | 0.0184 (2) | 0.0168 (2) | 0.0181 (2) | 0.00010 (18) | 0.00149 (17) | −0.00075 (19) |
P2 | 0.0200 (2) | 0.0171 (2) | 0.0161 (2) | 0.00133 (18) | 0.00102 (18) | −0.00062 (18) |
C1 | 0.0229 (9) | 0.0183 (9) | 0.0174 (9) | 0.0007 (7) | 0.0039 (7) | −0.0018 (7) |
C2 | 0.0254 (10) | 0.0208 (10) | 0.0203 (9) | 0.0004 (8) | 0.0008 (8) | −0.0021 (8) |
C3 | 0.0301 (11) | 0.0234 (10) | 0.0298 (11) | −0.0063 (9) | 0.0065 (9) | −0.0060 (9) |
C4 | 0.0405 (12) | 0.0187 (10) | 0.0316 (11) | −0.0029 (9) | 0.0127 (10) | −0.0009 (9) |
C5 | 0.0367 (12) | 0.0271 (11) | 0.0290 (11) | 0.0073 (9) | 0.0057 (9) | 0.0084 (9) |
C6 | 0.0255 (10) | 0.0262 (11) | 0.0252 (10) | 0.0018 (9) | 0.0011 (8) | 0.0015 (9) |
C7 | 0.0190 (9) | 0.0208 (9) | 0.0225 (10) | −0.0001 (8) | 0.0013 (7) | 0.0014 (8) |
C8 | 0.0246 (10) | 0.0381 (13) | 0.0328 (12) | 0.0010 (9) | 0.0013 (9) | −0.0121 (10) |
C9 | 0.0216 (10) | 0.0466 (14) | 0.0386 (13) | 0.0052 (10) | 0.0046 (9) | −0.0081 (11) |
C10 | 0.0188 (10) | 0.0371 (13) | 0.0460 (14) | −0.0015 (9) | −0.0016 (9) | 0.0031 (11) |
C11 | 0.0284 (12) | 0.0353 (13) | 0.0598 (17) | −0.0012 (10) | −0.0122 (11) | −0.0151 (12) |
C12 | 0.0252 (11) | 0.0292 (12) | 0.0435 (13) | 0.0023 (9) | −0.0049 (10) | −0.0120 (10) |
C13 | 0.0195 (9) | 0.0231 (10) | 0.0192 (9) | 0.0000 (8) | 0.0003 (7) | 0.0000 (8) |
C14 | 0.0399 (12) | 0.0258 (11) | 0.0246 (11) | 0.0063 (10) | −0.0026 (9) | −0.0018 (9) |
C15 | 0.0627 (17) | 0.0290 (12) | 0.0253 (11) | 0.0135 (12) | −0.0036 (11) | 0.0047 (10) |
C16 | 0.0493 (14) | 0.0411 (14) | 0.0188 (10) | 0.0123 (12) | −0.0026 (10) | −0.0002 (10) |
C17 | 0.0390 (12) | 0.0316 (12) | 0.0221 (10) | 0.0050 (10) | 0.0008 (9) | −0.0068 (9) |
C18 | 0.0304 (11) | 0.0226 (10) | 0.0246 (10) | 0.0008 (9) | 0.0019 (8) | −0.0012 (8) |
C19 | 0.0223 (9) | 0.0194 (9) | 0.0199 (9) | −0.0025 (8) | −0.0023 (7) | −0.0002 (8) |
C20 | 0.0298 (11) | 0.0329 (12) | 0.0257 (11) | 0.0081 (9) | −0.0003 (8) | −0.0018 (9) |
C21 | 0.0306 (11) | 0.0356 (13) | 0.0360 (13) | 0.0072 (10) | −0.0064 (10) | 0.0012 (10) |
C22 | 0.0357 (12) | 0.0346 (12) | 0.0277 (11) | −0.0025 (10) | −0.0110 (9) | 0.0031 (10) |
C23 | 0.0371 (12) | 0.0375 (13) | 0.0200 (10) | −0.0026 (10) | −0.0026 (9) | −0.0009 (9) |
C24 | 0.0251 (10) | 0.0272 (11) | 0.0223 (10) | 0.0008 (8) | 0.0004 (8) | −0.0006 (8) |
C25 | 0.0232 (9) | 0.0218 (9) | 0.0143 (9) | 0.0041 (8) | 0.0003 (7) | −0.0015 (8) |
C26 | 0.0282 (10) | 0.0255 (10) | 0.0203 (10) | 0.0009 (9) | 0.0003 (8) | −0.0025 (8) |
C27 | 0.0459 (13) | 0.0222 (10) | 0.0245 (11) | 0.0041 (10) | 0.0007 (9) | −0.0047 (9) |
C28 | 0.0396 (12) | 0.0320 (12) | 0.0216 (10) | 0.0164 (10) | −0.0010 (9) | −0.0042 (9) |
C29 | 0.0254 (10) | 0.0388 (13) | 0.0227 (10) | 0.0102 (9) | −0.0012 (8) | −0.0029 (9) |
C30 | 0.0258 (10) | 0.0253 (10) | 0.0215 (10) | 0.0021 (8) | 0.0002 (8) | −0.0015 (8) |
C31 | 0.0212 (9) | 0.0197 (9) | 0.0173 (9) | 0.0010 (8) | 0.0025 (7) | −0.0034 (7) |
C32 | 0.0277 (10) | 0.0238 (10) | 0.0196 (10) | 0.0001 (8) | 0.0004 (8) | −0.0021 (8) |
C33 | 0.0345 (11) | 0.0214 (10) | 0.0312 (11) | −0.0034 (9) | 0.0047 (9) | −0.0007 (9) |
C34 | 0.0272 (11) | 0.0286 (11) | 0.0369 (12) | −0.0049 (9) | 0.0024 (9) | −0.0127 (10) |
C35 | 0.0290 (11) | 0.0348 (12) | 0.0249 (10) | 0.0032 (9) | −0.0046 (8) | −0.0091 (9) |
C36 | 0.0272 (10) | 0.0254 (10) | 0.0208 (10) | 0.0039 (8) | −0.0004 (8) | −0.0017 (8) |
O40 | 0.090 (2) | 0.081 (2) | 0.134 (3) | −0.0056 (17) | 0.042 (2) | 0.034 (2) |
C41 | 0.164 (6) | 0.097 (4) | 0.179 (7) | 0.041 (4) | 0.075 (6) | 0.041 (4) |
C42 | 0.165 (6) | 0.144 (6) | 0.153 (6) | −0.024 (5) | 0.051 (5) | −0.110 (5) |
C43 | 0.132 (5) | 0.133 (5) | 0.090 (4) | 0.004 (4) | −0.031 (3) | 0.051 (4) |
C44 | 0.092 (3) | 0.080 (3) | 0.090 (3) | −0.002 (2) | 0.035 (3) | 0.001 (2) |
Geometric parameters (Å, º) top
Ni1—Cl1 | 2.1481 (6) | C20—C21 | 1.391 (3) |
Ni1—P2 | 2.2012 (6) | C20—H20 | 0.9500 |
Ni1—P1 | 2.2091 (6) | C21—C22 | 1.379 (3) |
P1—C1 | 1.817 (2) | C21—H21 | 0.9500 |
P1—C7 | 1.820 (2) | C22—C23 | 1.382 (3) |
P1—C13 | 1.828 (2) | C22—H22 | 0.9500 |
P2—C31 | 1.821 (2) | C23—C24 | 1.397 (3) |
P2—C19 | 1.828 (2) | C23—H23 | 0.9500 |
P2—C25 | 1.835 (2) | C24—H24 | 0.9500 |
C1—C2 | 1.395 (3) | C25—C30 | 1.395 (3) |
C1—C6 | 1.398 (3) | C25—C26 | 1.395 (3) |
C2—C3 | 1.387 (3) | C26—C27 | 1.387 (3) |
C2—H2 | 0.9500 | C26—H26 | 0.9500 |
C3—C4 | 1.387 (3) | C27—C28 | 1.384 (4) |
C3—H3 | 0.9500 | C27—H27 | 0.9500 |
C4—C5 | 1.386 (3) | C28—C29 | 1.382 (3) |
C4—H4 | 0.9500 | C28—H28 | 0.9500 |
C5—C6 | 1.387 (3) | C29—C30 | 1.391 (3) |
C5—H5 | 0.9500 | C29—H29 | 0.9500 |
C6—H6 | 0.9500 | C30—H30 | 0.9500 |
C7—C12 | 1.382 (3) | C31—C32 | 1.389 (3) |
C7—C8 | 1.395 (3) | C31—C36 | 1.396 (3) |
C8—C9 | 1.382 (3) | C32—C33 | 1.394 (3) |
C8—H8 | 0.9500 | C32—H32 | 0.9500 |
C9—C10 | 1.378 (3) | C33—C34 | 1.381 (3) |
C9—H9 | 0.9500 | C33—H33 | 0.9500 |
C10—C11 | 1.377 (4) | C34—C35 | 1.386 (3) |
C10—H10 | 0.9500 | C34—H34 | 0.9500 |
C11—C12 | 1.391 (3) | C35—C36 | 1.386 (3) |
C11—H11 | 0.9500 | C35—H35 | 0.9500 |
C12—H12 | 0.9500 | C36—H36 | 0.9500 |
C13—C14 | 1.394 (3) | O40—C44 | 1.315 (5) |
C13—C18 | 1.395 (3) | O40—C41 | 1.336 (6) |
C14—C15 | 1.389 (3) | C41—C42 | 1.515 (9) |
C14—H14 | 0.9500 | C41—H41A | 0.9900 |
C15—C16 | 1.385 (3) | C41—H41B | 0.9900 |
C15—H15 | 0.9500 | C42—C43 | 1.524 (8) |
C16—C17 | 1.384 (3) | C42—H42A | 0.9900 |
C16—H16 | 0.9500 | C42—H42B | 0.9900 |
C17—C18 | 1.390 (3) | C43—C44 | 1.521 (7) |
C17—H17 | 0.9500 | C43—H43A | 0.9900 |
C18—H18 | 0.9500 | C43—H43B | 0.9900 |
C19—C24 | 1.390 (3) | C44—H44A | 0.9900 |
C19—C20 | 1.392 (3) | C44—H44B | 0.9900 |
| | | |
Cl1—Ni1—P2 | 126.98 (2) | C19—C20—H20 | 119.7 |
Cl1—Ni1—P1 | 121.33 (2) | C22—C21—C20 | 119.8 (2) |
P2—Ni1—P1 | 111.52 (2) | C22—C21—H21 | 120.1 |
C1—P1—C7 | 103.73 (9) | C20—C21—H21 | 120.1 |
C1—P1—C13 | 103.92 (9) | C21—C22—C23 | 120.4 (2) |
C7—P1—C13 | 103.21 (9) | C21—C22—H22 | 119.8 |
C1—P1—Ni1 | 119.92 (6) | C23—C22—H22 | 119.8 |
C7—P1—Ni1 | 111.87 (7) | C22—C23—C24 | 119.9 (2) |
C13—P1—Ni1 | 112.51 (7) | C22—C23—H23 | 120.1 |
C31—P2—C19 | 104.62 (9) | C24—C23—H23 | 120.1 |
C31—P2—C25 | 102.30 (9) | C19—C24—C23 | 120.3 (2) |
C19—P2—C25 | 104.51 (9) | C19—C24—H24 | 119.8 |
C31—P2—Ni1 | 121.64 (6) | C23—C24—H24 | 119.8 |
C19—P2—Ni1 | 111.78 (7) | C30—C25—C26 | 118.87 (19) |
C25—P2—Ni1 | 110.37 (7) | C30—C25—P2 | 123.19 (16) |
C2—C1—C6 | 118.88 (19) | C26—C25—P2 | 117.88 (15) |
C2—C1—P1 | 118.33 (15) | C27—C26—C25 | 120.5 (2) |
C6—C1—P1 | 122.60 (16) | C27—C26—H26 | 119.8 |
C3—C2—C1 | 120.8 (2) | C25—C26—H26 | 119.8 |
C3—C2—H2 | 119.6 | C28—C27—C26 | 120.3 (2) |
C1—C2—H2 | 119.6 | C28—C27—H27 | 119.8 |
C4—C3—C2 | 120.0 (2) | C26—C27—H27 | 119.8 |
C4—C3—H3 | 120.0 | C29—C28—C27 | 119.6 (2) |
C2—C3—H3 | 120.0 | C29—C28—H28 | 120.2 |
C5—C4—C3 | 119.7 (2) | C27—C28—H28 | 120.2 |
C5—C4—H4 | 120.1 | C28—C29—C30 | 120.6 (2) |
C3—C4—H4 | 120.1 | C28—C29—H29 | 119.7 |
C4—C5—C6 | 120.6 (2) | C30—C29—H29 | 119.7 |
C4—C5—H5 | 119.7 | C29—C30—C25 | 120.1 (2) |
C6—C5—H5 | 119.7 | C29—C30—H30 | 119.9 |
C5—C6—C1 | 120.0 (2) | C25—C30—H30 | 119.9 |
C5—C6—H6 | 120.0 | C32—C31—C36 | 118.70 (19) |
C1—C6—H6 | 120.0 | C32—C31—P2 | 122.89 (15) |
C12—C7—C8 | 118.75 (19) | C36—C31—P2 | 118.36 (16) |
C12—C7—P1 | 119.24 (16) | C31—C32—C33 | 120.6 (2) |
C8—C7—P1 | 122.01 (16) | C31—C32—H32 | 119.7 |
C9—C8—C7 | 120.4 (2) | C33—C32—H32 | 119.7 |
C9—C8—H8 | 119.8 | C34—C33—C32 | 120.0 (2) |
C7—C8—H8 | 119.8 | C34—C33—H33 | 120.0 |
C10—C9—C8 | 120.4 (2) | C32—C33—H33 | 120.0 |
C10—C9—H9 | 119.8 | C33—C34—C35 | 120.0 (2) |
C8—C9—H9 | 119.8 | C33—C34—H34 | 120.0 |
C11—C10—C9 | 119.8 (2) | C35—C34—H34 | 120.0 |
C11—C10—H10 | 120.1 | C36—C35—C34 | 120.0 (2) |
C9—C10—H10 | 120.1 | C36—C35—H35 | 120.0 |
C10—C11—C12 | 120.1 (2) | C34—C35—H35 | 120.0 |
C10—C11—H11 | 119.9 | C35—C36—C31 | 120.7 (2) |
C12—C11—H11 | 119.9 | C35—C36—H36 | 119.7 |
C7—C12—C11 | 120.6 (2) | C31—C36—H36 | 119.7 |
C7—C12—H12 | 119.7 | C44—O40—C41 | 103.7 (4) |
C11—C12—H12 | 119.7 | O40—C41—C42 | 104.6 (5) |
C14—C13—C18 | 118.91 (19) | O40—C41—H41A | 110.8 |
C14—C13—P1 | 117.49 (15) | C42—C41—H41A | 110.8 |
C18—C13—P1 | 123.51 (16) | O40—C41—H41B | 110.8 |
C15—C14—C13 | 120.6 (2) | C42—C41—H41B | 110.8 |
C15—C14—H14 | 119.7 | H41A—C41—H41B | 108.9 |
C13—C14—H14 | 119.7 | C41—C42—C43 | 101.1 (4) |
C16—C15—C14 | 120.0 (2) | C41—C42—H42A | 111.6 |
C16—C15—H15 | 120.0 | C43—C42—H42A | 111.6 |
C14—C15—H15 | 120.0 | C41—C42—H42B | 111.6 |
C17—C16—C15 | 120.0 (2) | C43—C42—H42B | 111.6 |
C17—C16—H16 | 120.0 | H42A—C42—H42B | 109.4 |
C15—C16—H16 | 120.0 | C44—C43—C42 | 100.1 (4) |
C16—C17—C18 | 120.2 (2) | C44—C43—H43A | 111.7 |
C16—C17—H17 | 119.9 | C42—C43—H43A | 111.7 |
C18—C17—H17 | 119.9 | C44—C43—H43B | 111.7 |
C17—C18—C13 | 120.3 (2) | C42—C43—H43B | 111.7 |
C17—C18—H18 | 119.8 | H43A—C43—H43B | 109.5 |
C13—C18—H18 | 119.8 | O40—C44—C43 | 106.6 (4) |
C24—C19—C20 | 118.94 (19) | O40—C44—H44A | 110.4 |
C24—C19—P2 | 122.84 (16) | C43—C44—H44A | 110.4 |
C20—C19—P2 | 118.21 (15) | O40—C44—H44B | 110.4 |
C21—C20—C19 | 120.7 (2) | C43—C44—H44B | 110.4 |
C21—C20—H20 | 119.7 | H44A—C44—H44B | 108.6 |
| | | |
Cl1—Ni1—P1—C1 | 176.45 (8) | C16—C17—C18—C13 | 0.3 (4) |
P2—Ni1—P1—C1 | 0.80 (8) | C14—C13—C18—C17 | 0.7 (3) |
Cl1—Ni1—P1—C7 | 54.70 (8) | P1—C13—C18—C17 | −175.74 (17) |
P2—Ni1—P1—C7 | −120.95 (7) | C31—P2—C19—C24 | −94.28 (18) |
Cl1—Ni1—P1—C13 | −60.95 (8) | C25—P2—C19—C24 | 12.9 (2) |
P2—Ni1—P1—C13 | 123.41 (7) | Ni1—P2—C19—C24 | 132.25 (16) |
Cl1—Ni1—P2—C31 | 143.72 (8) | C31—P2—C19—C20 | 85.77 (18) |
P1—Ni1—P2—C31 | −40.93 (8) | C25—P2—C19—C20 | −167.08 (17) |
Cl1—Ni1—P2—C19 | −91.84 (8) | Ni1—P2—C19—C20 | −47.71 (18) |
P1—Ni1—P2—C19 | 83.50 (7) | C24—C19—C20—C21 | 1.1 (3) |
Cl1—Ni1—P2—C25 | 24.01 (8) | P2—C19—C20—C21 | −178.92 (18) |
P1—Ni1—P2—C25 | −160.65 (7) | C19—C20—C21—C22 | −0.8 (4) |
C7—P1—C1—C2 | −162.60 (15) | C20—C21—C22—C23 | −0.4 (4) |
C13—P1—C1—C2 | −54.97 (17) | C21—C22—C23—C24 | 1.1 (4) |
Ni1—P1—C1—C2 | 71.74 (17) | C20—C19—C24—C23 | −0.4 (3) |
C7—P1—C1—C6 | 22.37 (19) | P2—C19—C24—C23 | 179.68 (17) |
C13—P1—C1—C6 | 130.00 (17) | C22—C23—C24—C19 | −0.7 (3) |
Ni1—P1—C1—C6 | −103.30 (16) | C31—P2—C25—C30 | 8.10 (19) |
C6—C1—C2—C3 | −0.3 (3) | C19—P2—C25—C30 | −100.76 (18) |
P1—C1—C2—C3 | −175.56 (15) | Ni1—P2—C25—C30 | 138.92 (16) |
C1—C2—C3—C4 | 0.7 (3) | C31—P2—C25—C26 | −169.04 (16) |
C2—C3—C4—C5 | −0.7 (3) | C19—P2—C25—C26 | 82.10 (17) |
C3—C4—C5—C6 | 0.3 (3) | Ni1—P2—C25—C26 | −38.22 (17) |
C4—C5—C6—C1 | 0.1 (3) | C30—C25—C26—C27 | −0.5 (3) |
C2—C1—C6—C5 | −0.1 (3) | P2—C25—C26—C27 | 176.76 (16) |
P1—C1—C6—C5 | 174.93 (16) | C25—C26—C27—C28 | −1.0 (3) |
C1—P1—C7—C12 | −121.82 (19) | C26—C27—C28—C29 | 1.5 (3) |
C13—P1—C7—C12 | 130.02 (19) | C27—C28—C29—C30 | −0.5 (3) |
Ni1—P1—C7—C12 | 8.8 (2) | C28—C29—C30—C25 | −1.1 (3) |
C1—P1—C7—C8 | 57.8 (2) | C26—C25—C30—C29 | 1.6 (3) |
C13—P1—C7—C8 | −50.3 (2) | P2—C25—C30—C29 | −175.56 (16) |
Ni1—P1—C7—C8 | −171.54 (17) | C19—P2—C31—C32 | 1.69 (19) |
C12—C7—C8—C9 | 1.3 (4) | C25—P2—C31—C32 | −107.08 (17) |
P1—C7—C8—C9 | −178.37 (19) | Ni1—P2—C31—C32 | 129.36 (15) |
C7—C8—C9—C10 | −0.7 (4) | C19—P2—C31—C36 | 179.10 (16) |
C8—C9—C10—C11 | −0.2 (4) | C25—P2—C31—C36 | 70.33 (17) |
C9—C10—C11—C12 | 0.5 (4) | Ni1—P2—C31—C36 | −53.23 (18) |
C8—C7—C12—C11 | −1.0 (4) | C36—C31—C32—C33 | −1.0 (3) |
P1—C7—C12—C11 | 178.7 (2) | P2—C31—C32—C33 | 176.39 (16) |
C10—C11—C12—C7 | 0.1 (4) | C31—C32—C33—C34 | −0.7 (3) |
C1—P1—C13—C14 | 158.28 (17) | C32—C33—C34—C35 | 1.4 (3) |
C7—P1—C13—C14 | −93.69 (18) | C33—C34—C35—C36 | −0.6 (3) |
Ni1—P1—C13—C14 | 27.07 (18) | C34—C35—C36—C31 | −1.1 (3) |
C1—P1—C13—C18 | −25.22 (19) | C32—C31—C36—C35 | 1.9 (3) |
C7—P1—C13—C18 | 82.80 (19) | P2—C31—C36—C35 | −175.62 (16) |
Ni1—P1—C13—C18 | −156.44 (16) | C44—O40—C41—C42 | 49.2 (7) |
C18—C13—C14—C15 | −1.4 (3) | O40—C41—C42—C43 | −31.0 (7) |
P1—C13—C14—C15 | 175.2 (2) | C41—C42—C43—C44 | 3.8 (6) |
C13—C14—C15—C16 | 1.1 (4) | C41—O40—C44—C43 | −47.0 (7) |
C14—C15—C16—C17 | −0.1 (4) | C42—C43—C44—O40 | 24.8 (6) |
C15—C16—C17—C18 | −0.6 (4) | | |
Crystal data top
[NiCl(C18H15P)3] | Dx = 1.341 Mg m−3 |
Mr = 880.97 | Mo Kα radiation, λ = 0.71073 Å |
Trigonal, P3 | Cell parameters from 25 reflections |
a = 19.0125 (8) Å | θ = 11.7–13.9° |
c = 10.4507 (7) Å | µ = 0.65 mm−1 |
V = 3271.6 (3) Å3 | T = 150 K |
Z = 3 | Block, yellow |
F(000) = 1377 | 0.50 × 0.25 × 0.25 mm |
Data collection top
Enraf-Nonius CAD4 diffractometer | Rint = 0.055 |
Radiation source: rotating anode | θmax = 27.5°, θmin = 1.2° |
Graphite monochromator | h = −24→23 |
w/2θ scans | k = −23→24 |
10742 measured reflections | l = −13→0 |
5286 independent reflections | 3 standard reflections every 60 min |
4500 reflections with I > 2σ(I) | intensity decay: <1% |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.031 | H-atom parameters constrained |
wR(F2) = 0.066 | w = 1/[σ2(Fo2) + (0.026P)2 + 0.0482P] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.001 |
5286 reflections | Δρmax = 0.30 e Å−3 |
533 parameters | Δρmin = −0.52 e Å−3 |
1 restraint | Absolute structure: see experimental |
Primary atom site location: heavy-atom method | |
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 | |
Ni1 | 0.0000 | 0.0000 | 0.59434 (8) | 0.01643 (15) | |
Cl1 | 0.0000 | 0.0000 | 0.37490 (13) | 0.0293 (3) | |
P1 | 0.03782 (5) | 0.12765 (5) | 0.67244 (8) | 0.01921 (17) | |
C111 | 0.14886 (19) | 0.19178 (19) | 0.6793 (3) | 0.0198 (6) | |
C112 | 0.1912 (2) | 0.2538 (2) | 0.7683 (3) | 0.0289 (8) | |
H112 | 0.1627 | 0.2649 | 0.8324 | 0.035* | |
C113 | 0.2753 (2) | 0.2989 (2) | 0.7620 (4) | 0.0349 (8) | |
H113 | 0.3041 | 0.3418 | 0.8212 | 0.042* | |
C114 | 0.3177 (2) | 0.2827 (2) | 0.6719 (4) | 0.0318 (8) | |
H114 | 0.3754 | 0.3130 | 0.6706 | 0.038* | |
C115 | 0.2760 (2) | 0.2221 (2) | 0.5832 (3) | 0.0318 (8) | |
H115 | 0.3050 | 0.2108 | 0.5202 | 0.038* | |
C116 | 0.1917 (2) | 0.1776 (2) | 0.5859 (3) | 0.0249 (7) | |
H116 | 0.1633 | 0.1370 | 0.5230 | 0.030* | |
C121 | 0.0029 (2) | 0.13179 (19) | 0.8351 (3) | 0.0204 (6) | |
C122 | 0.0417 (2) | 0.1209 (2) | 0.9398 (3) | 0.0253 (7) | |
H122 | 0.0900 | 0.1185 | 0.9280 | 0.030* | |
C123 | 0.0095 (2) | 0.1134 (2) | 1.0618 (3) | 0.0305 (8) | |
H123 | 0.0358 | 0.1057 | 1.1332 | 0.037* | |
C124 | −0.0602 (2) | 0.1172 (2) | 1.0798 (3) | 0.0332 (9) | |
H124 | −0.0817 | 0.1120 | 1.1635 | 0.040* | |
C125 | −0.0989 (2) | 0.1286 (2) | 0.9769 (3) | 0.0345 (8) | |
H125 | −0.1470 | 0.1313 | 0.9895 | 0.041* | |
C126 | −0.0668 (2) | 0.1361 (2) | 0.8537 (3) | 0.0259 (7) | |
H126 | −0.0931 | 0.1441 | 0.7826 | 0.031* | |
C131 | 0.0140 (2) | 0.1964 (2) | 0.5825 (3) | 0.0220 (7) | |
C132 | −0.0154 (2) | 0.1772 (2) | 0.4581 (3) | 0.0261 (7) | |
H132 | −0.0248 | 0.1278 | 0.4202 | 0.031* | |
C133 | −0.0312 (2) | 0.2303 (2) | 0.3891 (3) | 0.0328 (8) | |
H133 | −0.0529 | 0.2161 | 0.3051 | 0.039* | |
C134 | −0.0162 (2) | 0.3026 (2) | 0.4401 (3) | 0.0348 (9) | |
H134 | −0.0272 | 0.3383 | 0.3917 | 0.042* | |
C135 | 0.0151 (2) | 0.3235 (2) | 0.5631 (4) | 0.0333 (8) | |
H135 | 0.0261 | 0.3739 | 0.5990 | 0.040* | |
C136 | 0.0301 (2) | 0.2715 (2) | 0.6323 (3) | 0.0283 (8) | |
H136 | 0.0519 | 0.2865 | 0.7161 | 0.034* | |
Ni2 | 0.3333 | 0.6667 | 0.37294 (7) | 0.01646 (15) | |
Cl2 | 0.3333 | 0.6667 | 0.59166 (12) | 0.0279 (3) | |
P2 | 0.20882 (5) | 0.57495 (5) | 0.29165 (8) | 0.01965 (16) | |
C211 | 0.19351 (19) | 0.4716 (2) | 0.2867 (3) | 0.0207 (7) | |
C212 | 0.2248 (2) | 0.4488 (2) | 0.3882 (3) | 0.0298 (8) | |
H212 | 0.2550 | 0.4873 | 0.4529 | 0.036* | |
C213 | 0.2129 (2) | 0.3710 (3) | 0.3969 (4) | 0.0373 (9) | |
H213 | 0.2339 | 0.3559 | 0.4676 | 0.045* | |
C214 | 0.1700 (3) | 0.3153 (3) | 0.3012 (4) | 0.0401 (10) | |
H214 | 0.1623 | 0.2620 | 0.3055 | 0.048* | |
C215 | 0.1386 (2) | 0.3370 (2) | 0.2002 (4) | 0.0348 (9) | |
H215 | 0.1089 | 0.2984 | 0.1354 | 0.042* | |
C216 | 0.1500 (2) | 0.4149 (2) | 0.1921 (3) | 0.0285 (8) | |
H216 | 0.1282 | 0.4295 | 0.1219 | 0.034* | |
C221 | 0.11562 (19) | 0.5520 (2) | 0.3784 (3) | 0.0215 (6) | |
C222 | 0.1199 (2) | 0.5701 (2) | 0.5080 (3) | 0.0279 (7) | |
H222 | 0.1711 | 0.5982 | 0.5495 | 0.033* | |
C223 | 0.0490 (2) | 0.5471 (2) | 0.5768 (3) | 0.0342 (9) | |
H223 | 0.0523 | 0.5592 | 0.6656 | 0.041* | |
C224 | −0.0255 (2) | 0.5072 (2) | 0.5187 (4) | 0.0380 (9) | |
H224 | −0.0733 | 0.4927 | 0.5666 | 0.046* | |
C225 | −0.0309 (2) | 0.4880 (2) | 0.3887 (4) | 0.0336 (8) | |
H225 | −0.0825 | 0.4597 | 0.3481 | 0.040* | |
C226 | 0.0387 (2) | 0.5101 (2) | 0.3195 (3) | 0.0273 (7) | |
H226 | 0.0348 | 0.4969 | 0.2312 | 0.033* | |
C231 | 0.18691 (19) | 0.5962 (2) | 0.1295 (3) | 0.0217 (6) | |
C232 | 0.1484 (2) | 0.6415 (2) | 0.1136 (3) | 0.0247 (7) | |
H232 | 0.1280 | 0.6558 | 0.1860 | 0.030* | |
C233 | 0.1398 (2) | 0.6660 (2) | −0.0083 (3) | 0.0319 (8) | |
H233 | 0.1133 | 0.6968 | −0.0185 | 0.038* | |
C234 | 0.1694 (2) | 0.6459 (2) | −0.1141 (3) | 0.0328 (8) | |
H234 | 0.1633 | 0.6628 | −0.1970 | 0.039* | |
C235 | 0.2078 (2) | 0.6012 (2) | −0.0993 (3) | 0.0288 (7) | |
H235 | 0.2283 | 0.5873 | −0.1721 | 0.035* | |
C236 | 0.2168 (2) | 0.5765 (2) | 0.0220 (3) | 0.0251 (7) | |
H236 | 0.2436 | 0.5459 | 0.0315 | 0.030* | |
Ni3 | 0.6667 | 0.3333 | 1.07600 (7) | 0.01592 (14) | |
Cl3 | 0.6667 | 0.3333 | 1.29591 (12) | 0.0285 (3) | |
P3 | 0.56358 (5) | 0.35084 (5) | 0.99768 (8) | 0.01946 (17) | |
C311 | 0.52501 (19) | 0.30644 (19) | 0.8395 (3) | 0.0187 (6) | |
C312 | 0.4591 (2) | 0.2286 (2) | 0.8268 (3) | 0.0253 (7) | |
H312 | 0.4281 | 0.2011 | 0.9003 | 0.030* | |
C313 | 0.4376 (2) | 0.1902 (2) | 0.7085 (3) | 0.0293 (7) | |
H313 | 0.3927 | 0.1366 | 0.7015 | 0.035* | |
C314 | 0.4818 (2) | 0.2302 (2) | 0.6011 (3) | 0.0303 (8) | |
H314 | 0.4675 | 0.2039 | 0.5202 | 0.036* | |
C315 | 0.5470 (2) | 0.3085 (2) | 0.6109 (3) | 0.0270 (7) | |
H315 | 0.5768 | 0.3362 | 0.5365 | 0.032* | |
C316 | 0.5690 (2) | 0.3469 (2) | 0.7298 (3) | 0.0223 (7) | |
H316 | 0.6139 | 0.4005 | 0.7363 | 0.027* | |
C321 | 0.47072 (19) | 0.3140 (2) | 1.0940 (3) | 0.0208 (7) | |
C322 | 0.4683 (2) | 0.2867 (3) | 1.2171 (3) | 0.0362 (9) | |
H322 | 0.5134 | 0.2840 | 1.2503 | 0.043* | |
C323 | 0.3999 (3) | 0.2632 (4) | 1.2924 (4) | 0.0555 (14) | |
H323 | 0.3986 | 0.2443 | 1.3770 | 0.067* | |
C324 | 0.3341 (2) | 0.2669 (3) | 1.2458 (3) | 0.0381 (9) | |
H324 | 0.2876 | 0.2509 | 1.2981 | 0.046* | |
C325 | 0.3360 (2) | 0.2935 (2) | 1.1247 (3) | 0.0331 (8) | |
H325 | 0.2907 | 0.2962 | 1.0923 | 0.040* | |
C326 | 0.4038 (2) | 0.3170 (3) | 1.0480 (3) | 0.0337 (9) | |
H326 | 0.4043 | 0.3353 | 0.9632 | 0.040* | |
C331 | 0.5903 (2) | 0.4578 (2) | 0.9835 (3) | 0.0223 (7) | |
C332 | 0.5613 (2) | 0.4882 (2) | 0.8894 (3) | 0.0297 (8) | |
H332 | 0.5246 | 0.4527 | 0.8266 | 0.036* | |
C333 | 0.5855 (3) | 0.5698 (3) | 0.8865 (4) | 0.0398 (10) | |
H333 | 0.5651 | 0.5900 | 0.8218 | 0.048* | |
C334 | 0.6391 (3) | 0.6224 (3) | 0.9771 (4) | 0.0451 (11) | |
H334 | 0.6576 | 0.6789 | 0.9721 | 0.054* | |
C335 | 0.6654 (3) | 0.5927 (2) | 1.0738 (4) | 0.0425 (10) | |
H335 | 0.7003 | 0.6282 | 1.1383 | 0.051* | |
C336 | 0.6409 (2) | 0.5103 (2) | 1.0773 (3) | 0.0332 (8) | |
H336 | 0.6592 | 0.4899 | 1.1448 | 0.040* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0179 (2) | 0.0179 (2) | 0.0135 (3) | 0.00895 (11) | 0.000 | 0.000 |
Cl1 | 0.0367 (5) | 0.0367 (5) | 0.0145 (7) | 0.0183 (3) | 0.000 | 0.000 |
P1 | 0.0218 (4) | 0.0197 (4) | 0.0168 (4) | 0.0109 (3) | −0.0005 (3) | −0.0015 (3) |
C111 | 0.0195 (16) | 0.0175 (16) | 0.0209 (16) | 0.0082 (13) | 0.0011 (13) | 0.0017 (12) |
C112 | 0.0305 (19) | 0.0280 (19) | 0.0294 (18) | 0.0156 (16) | −0.0015 (15) | −0.0064 (15) |
C113 | 0.033 (2) | 0.029 (2) | 0.042 (2) | 0.0154 (17) | −0.0076 (17) | −0.0087 (16) |
C114 | 0.0185 (17) | 0.0277 (19) | 0.044 (2) | 0.0079 (15) | 0.0001 (15) | 0.0068 (16) |
C115 | 0.032 (2) | 0.038 (2) | 0.0273 (18) | 0.0190 (17) | 0.0104 (15) | 0.0057 (15) |
C116 | 0.0305 (19) | 0.0254 (18) | 0.0175 (15) | 0.0129 (16) | 0.0023 (13) | 0.0022 (13) |
C121 | 0.0263 (17) | 0.0178 (15) | 0.0187 (15) | 0.0123 (14) | 0.0010 (13) | −0.0012 (12) |
C122 | 0.0297 (18) | 0.0242 (17) | 0.0204 (16) | 0.0123 (15) | −0.0013 (13) | −0.0024 (13) |
C123 | 0.040 (2) | 0.035 (2) | 0.0153 (15) | 0.0184 (18) | −0.0030 (14) | −0.0040 (14) |
C124 | 0.046 (2) | 0.031 (2) | 0.0195 (17) | 0.0172 (18) | 0.0071 (16) | −0.0059 (14) |
C125 | 0.034 (2) | 0.040 (2) | 0.037 (2) | 0.0240 (19) | 0.0077 (16) | −0.0009 (16) |
C126 | 0.0286 (19) | 0.0279 (19) | 0.0231 (16) | 0.0155 (16) | 0.0013 (14) | −0.0019 (14) |
C131 | 0.0196 (16) | 0.0232 (16) | 0.0234 (16) | 0.0109 (14) | 0.0032 (12) | 0.0053 (13) |
C132 | 0.0298 (19) | 0.0263 (18) | 0.0225 (17) | 0.0142 (16) | 0.0012 (14) | 0.0008 (13) |
C133 | 0.042 (2) | 0.037 (2) | 0.0213 (17) | 0.0212 (18) | −0.0020 (15) | 0.0025 (15) |
C134 | 0.045 (2) | 0.036 (2) | 0.0331 (19) | 0.0268 (19) | 0.0073 (17) | 0.0133 (16) |
C135 | 0.044 (2) | 0.0267 (19) | 0.0343 (19) | 0.0219 (18) | 0.0065 (16) | 0.0019 (15) |
C136 | 0.037 (2) | 0.0247 (18) | 0.0237 (17) | 0.0153 (16) | −0.0022 (14) | −0.0045 (14) |
Ni2 | 0.0175 (2) | 0.0175 (2) | 0.0145 (3) | 0.00873 (10) | 0.000 | 0.000 |
Cl2 | 0.0349 (5) | 0.0349 (5) | 0.0138 (6) | 0.0174 (3) | 0.000 | 0.000 |
P2 | 0.0178 (4) | 0.0217 (4) | 0.0171 (4) | 0.0082 (3) | −0.0007 (3) | −0.0008 (3) |
C211 | 0.0190 (16) | 0.0217 (16) | 0.0206 (16) | 0.0095 (14) | 0.0058 (13) | 0.0022 (13) |
C212 | 0.0228 (18) | 0.0316 (19) | 0.0331 (18) | 0.0120 (16) | 0.0016 (15) | 0.0028 (15) |
C213 | 0.034 (2) | 0.041 (2) | 0.043 (2) | 0.0232 (19) | 0.0045 (17) | 0.0132 (18) |
C214 | 0.033 (2) | 0.029 (2) | 0.063 (3) | 0.0188 (18) | 0.0109 (19) | 0.0080 (19) |
C215 | 0.030 (2) | 0.0233 (18) | 0.046 (2) | 0.0097 (16) | 0.0015 (17) | −0.0096 (16) |
C216 | 0.0236 (18) | 0.0242 (18) | 0.0344 (19) | 0.0094 (15) | 0.0005 (15) | −0.0023 (15) |
C221 | 0.0180 (16) | 0.0228 (17) | 0.0227 (15) | 0.0095 (14) | 0.0034 (12) | 0.0017 (13) |
C222 | 0.0240 (17) | 0.0290 (18) | 0.0249 (16) | 0.0089 (15) | −0.0014 (13) | −0.0028 (14) |
C223 | 0.037 (2) | 0.036 (2) | 0.0271 (18) | 0.0167 (18) | 0.0095 (16) | −0.0042 (15) |
C224 | 0.029 (2) | 0.039 (2) | 0.046 (2) | 0.0171 (18) | 0.0115 (17) | −0.0045 (18) |
C225 | 0.0209 (18) | 0.035 (2) | 0.043 (2) | 0.0125 (16) | −0.0002 (16) | −0.0044 (17) |
C226 | 0.0237 (17) | 0.0278 (18) | 0.0265 (17) | 0.0100 (15) | −0.0027 (14) | −0.0044 (14) |
C231 | 0.0195 (16) | 0.0240 (17) | 0.0191 (15) | 0.0091 (14) | −0.0034 (12) | −0.0024 (12) |
C232 | 0.0227 (17) | 0.0286 (18) | 0.0231 (16) | 0.0132 (15) | −0.0034 (13) | −0.0028 (14) |
C233 | 0.0288 (19) | 0.037 (2) | 0.0339 (19) | 0.0196 (17) | −0.0085 (15) | −0.0011 (16) |
C234 | 0.035 (2) | 0.039 (2) | 0.0189 (16) | 0.0149 (18) | −0.0084 (15) | −0.0008 (15) |
C235 | 0.0313 (19) | 0.035 (2) | 0.0201 (15) | 0.0169 (17) | −0.0023 (14) | −0.0043 (14) |
C236 | 0.0183 (16) | 0.0258 (17) | 0.0287 (17) | 0.0092 (14) | −0.0006 (13) | −0.0019 (14) |
Ni3 | 0.0182 (2) | 0.0182 (2) | 0.0114 (3) | 0.00910 (11) | 0.000 | 0.000 |
Cl3 | 0.0371 (5) | 0.0371 (5) | 0.0113 (6) | 0.0186 (3) | 0.000 | 0.000 |
P3 | 0.0180 (4) | 0.0249 (4) | 0.0161 (4) | 0.0112 (3) | 0.0006 (3) | 0.0022 (3) |
C311 | 0.0220 (16) | 0.0228 (16) | 0.0153 (14) | 0.0142 (14) | −0.0013 (12) | 0.0011 (12) |
C312 | 0.0210 (16) | 0.0270 (18) | 0.0275 (17) | 0.0118 (15) | −0.0025 (13) | 0.0042 (14) |
C313 | 0.0280 (18) | 0.0236 (18) | 0.0358 (19) | 0.0124 (15) | −0.0073 (15) | −0.0043 (14) |
C314 | 0.040 (2) | 0.038 (2) | 0.0244 (17) | 0.0280 (18) | −0.0125 (15) | −0.0076 (15) |
C315 | 0.036 (2) | 0.037 (2) | 0.0191 (16) | 0.0258 (18) | 0.0015 (14) | 0.0030 (14) |
C316 | 0.0197 (16) | 0.0260 (17) | 0.0244 (17) | 0.0137 (14) | 0.0010 (13) | 0.0022 (13) |
C321 | 0.0166 (15) | 0.0255 (17) | 0.0193 (15) | 0.0097 (14) | 0.0029 (12) | 0.0016 (13) |
C322 | 0.032 (2) | 0.065 (3) | 0.0206 (17) | 0.031 (2) | 0.0039 (15) | 0.0072 (17) |
C323 | 0.049 (3) | 0.112 (5) | 0.0247 (19) | 0.055 (3) | 0.0149 (18) | 0.027 (2) |
C324 | 0.034 (2) | 0.061 (3) | 0.0299 (19) | 0.031 (2) | 0.0110 (16) | 0.0098 (18) |
C325 | 0.0268 (19) | 0.045 (2) | 0.0336 (19) | 0.0230 (18) | 0.0029 (15) | 0.0083 (17) |
C326 | 0.035 (2) | 0.050 (2) | 0.0232 (17) | 0.0261 (19) | 0.0057 (15) | 0.0157 (16) |
C331 | 0.0221 (17) | 0.0230 (16) | 0.0220 (16) | 0.0113 (14) | 0.0062 (13) | −0.0008 (13) |
C332 | 0.0303 (19) | 0.0322 (19) | 0.0311 (18) | 0.0190 (16) | 0.0044 (15) | 0.0016 (15) |
C333 | 0.043 (2) | 0.034 (2) | 0.049 (2) | 0.024 (2) | 0.0167 (19) | 0.0092 (18) |
C334 | 0.053 (3) | 0.026 (2) | 0.055 (3) | 0.018 (2) | 0.025 (2) | 0.0014 (18) |
C335 | 0.039 (2) | 0.035 (2) | 0.040 (2) | 0.0075 (19) | 0.0119 (18) | −0.0171 (18) |
C336 | 0.031 (2) | 0.039 (2) | 0.0254 (18) | 0.0143 (17) | 0.0066 (15) | −0.0056 (16) |
Geometric parameters (Å, º) top
Ni1—Cl1 | 2.2933 (17) | C222—C223 | 1.392 (5) |
Ni1—P1i | 2.3082 (9) | C222—H222 | 0.9500 |
Ni1—P1 | 2.3082 (9) | C223—C224 | 1.369 (6) |
Ni1—P1ii | 2.3083 (9) | C223—H223 | 0.9500 |
P1—C111 | 1.837 (3) | C224—C225 | 1.398 (5) |
P1—C131 | 1.841 (3) | C224—H224 | 0.9500 |
P1—C121 | 1.840 (3) | C225—C226 | 1.376 (5) |
C111—C116 | 1.382 (4) | C225—H225 | 0.9500 |
C111—C112 | 1.398 (5) | C226—H226 | 0.9500 |
C112—C113 | 1.388 (5) | C231—C232 | 1.391 (5) |
C112—H112 | 0.9500 | C231—C236 | 1.393 (4) |
C113—C114 | 1.371 (5) | C232—C233 | 1.395 (5) |
C113—H113 | 0.9500 | C232—H232 | 0.9500 |
C114—C115 | 1.379 (5) | C233—C234 | 1.378 (5) |
C114—H114 | 0.9500 | C233—H233 | 0.9500 |
C115—C116 | 1.389 (5) | C234—C235 | 1.380 (5) |
C115—H115 | 0.9500 | C234—H234 | 0.9500 |
C116—H116 | 0.9500 | C235—C236 | 1.392 (5) |
C121—C126 | 1.381 (5) | C235—H235 | 0.9500 |
C121—C122 | 1.392 (5) | C236—H236 | 0.9500 |
C122—C123 | 1.390 (5) | Ni3—P3v | 2.2966 (9) |
C122—H122 | 0.9500 | Ni3—P3vi | 2.2966 (9) |
C123—C124 | 1.375 (5) | Ni3—P3 | 2.2966 (9) |
C123—H123 | 0.9500 | Ni3—Cl3 | 2.2982 (16) |
C124—C125 | 1.379 (5) | P3—C311 | 1.834 (3) |
C124—H124 | 0.9500 | P3—C331 | 1.838 (3) |
C125—C126 | 1.402 (5) | P3—C321 | 1.839 (3) |
C125—H125 | 0.9500 | C311—C312 | 1.387 (5) |
C126—H126 | 0.9500 | C311—C316 | 1.401 (4) |
C131—C132 | 1.390 (5) | C312—C313 | 1.389 (5) |
C131—C136 | 1.401 (5) | C312—H312 | 0.9500 |
C132—C133 | 1.391 (5) | C313—C314 | 1.381 (5) |
C132—H132 | 0.9500 | C313—H313 | 0.9500 |
C133—C134 | 1.363 (5) | C314—C315 | 1.385 (5) |
C133—H133 | 0.9500 | C314—H314 | 0.9500 |
C134—C135 | 1.389 (5) | C315—C316 | 1.395 (5) |
C134—H134 | 0.9500 | C315—H315 | 0.9500 |
C135—C136 | 1.366 (5) | C316—H316 | 0.9500 |
C135—H135 | 0.9500 | C321—C322 | 1.380 (5) |
C136—H136 | 0.9500 | C321—C326 | 1.388 (5) |
Ni2—Cl2 | 2.2858 (16) | C322—C323 | 1.388 (5) |
Ni2—P2iii | 2.2887 (9) | C322—H322 | 0.9500 |
Ni2—P2 | 2.2887 (9) | C323—C324 | 1.379 (5) |
Ni2—P2iv | 2.2888 (9) | C323—H323 | 0.9500 |
P2—C211 | 1.837 (3) | C324—C325 | 1.356 (5) |
P2—C231 | 1.837 (3) | C324—H324 | 0.9500 |
P2—C221 | 1.838 (3) | C325—C326 | 1.388 (5) |
C211—C212 | 1.388 (5) | C325—H325 | 0.9500 |
C211—C216 | 1.390 (5) | C326—H326 | 0.9500 |
C212—C213 | 1.383 (5) | C331—C336 | 1.387 (5) |
C212—H212 | 0.9500 | C331—C332 | 1.388 (5) |
C213—C214 | 1.387 (6) | C332—C333 | 1.380 (5) |
C213—H213 | 0.9500 | C332—H332 | 0.9500 |
C214—C215 | 1.373 (6) | C333—C334 | 1.385 (6) |
C214—H214 | 0.9500 | C333—H333 | 0.9500 |
C215—C216 | 1.387 (5) | C334—C335 | 1.368 (6) |
C215—H215 | 0.9500 | C334—H334 | 0.9500 |
C216—H216 | 0.9500 | C335—C336 | 1.394 (6) |
C221—C222 | 1.390 (4) | C335—H335 | 0.9500 |
C221—C226 | 1.410 (5) | C336—H336 | 0.9500 |
| | | |
Cl1—Ni1—P1i | 110.71 (3) | C221—C222—C223 | 119.9 (3) |
Cl1—Ni1—P1 | 110.71 (3) | C221—C222—H222 | 120.1 |
P1i—Ni1—P1 | 108.21 (3) | C223—C222—H222 | 120.1 |
Cl1—Ni1—P1ii | 110.71 (3) | C224—C223—C222 | 121.0 (3) |
P1i—Ni1—P1ii | 108.21 (3) | C224—C223—H223 | 119.5 |
P1—Ni1—P1ii | 108.21 (3) | C222—C223—H223 | 119.5 |
C111—P1—C131 | 99.05 (15) | C223—C224—C225 | 119.8 (3) |
C111—P1—C121 | 104.77 (15) | C223—C224—H224 | 120.1 |
C131—P1—C121 | 102.66 (15) | C225—C224—H224 | 120.1 |
C111—P1—Ni1 | 111.23 (11) | C226—C225—C224 | 119.8 (3) |
C131—P1—Ni1 | 120.55 (11) | C226—C225—H225 | 120.1 |
C121—P1—Ni1 | 116.24 (11) | C224—C225—H225 | 120.1 |
C116—C111—C112 | 119.2 (3) | C225—C226—C221 | 120.7 (3) |
C116—C111—P1 | 115.9 (2) | C225—C226—H226 | 119.6 |
C112—C111—P1 | 124.9 (3) | C221—C226—H226 | 119.6 |
C113—C112—C111 | 119.3 (3) | C232—C231—C236 | 118.8 (3) |
C113—C112—H112 | 120.4 | C232—C231—P2 | 119.6 (2) |
C111—C112—H112 | 120.4 | C236—C231—P2 | 121.1 (3) |
C114—C113—C112 | 121.3 (3) | C231—C232—C233 | 120.1 (3) |
C114—C113—H113 | 119.4 | C231—C232—H232 | 119.9 |
C112—C113—H113 | 119.4 | C233—C232—H232 | 119.9 |
C113—C114—C115 | 119.5 (3) | C234—C233—C232 | 120.6 (3) |
C113—C114—H114 | 120.3 | C234—C233—H233 | 119.7 |
C115—C114—H114 | 120.3 | C232—C233—H233 | 119.7 |
C114—C115—C116 | 120.1 (3) | C233—C234—C235 | 119.7 (3) |
C114—C115—H115 | 119.9 | C233—C234—H234 | 120.1 |
C116—C115—H115 | 119.9 | C235—C234—H234 | 120.1 |
C111—C116—C115 | 120.5 (3) | C234—C235—C236 | 120.2 (3) |
C111—C116—H116 | 119.7 | C234—C235—H235 | 119.9 |
C115—C116—H116 | 119.7 | C236—C235—H235 | 119.9 |
C126—C121—C122 | 119.5 (3) | C235—C236—C231 | 120.6 (3) |
C126—C121—P1 | 120.6 (2) | C235—C236—H236 | 119.7 |
C122—C121—P1 | 119.4 (2) | C231—C236—H236 | 119.7 |
C123—C122—C121 | 119.8 (3) | P3v—Ni3—P3vi | 108.03 (3) |
C123—C122—H122 | 120.1 | P3v—Ni3—P3 | 108.03 (3) |
C121—C122—H122 | 120.1 | P3vi—Ni3—P3 | 108.03 (3) |
C124—C123—C122 | 120.4 (3) | P3v—Ni3—Cl3 | 110.88 (3) |
C124—C123—H123 | 119.8 | P3vi—Ni3—Cl3 | 110.88 (3) |
C122—C123—H123 | 119.8 | P3—Ni3—Cl3 | 110.88 (3) |
C123—C124—C125 | 120.4 (3) | C311—P3—C331 | 105.19 (14) |
C123—C124—H124 | 119.8 | C311—P3—C321 | 103.36 (14) |
C125—C124—H124 | 119.8 | C331—P3—C321 | 98.47 (15) |
C124—C125—C126 | 119.4 (3) | C311—P3—Ni3 | 115.36 (10) |
C124—C125—H125 | 120.3 | C331—P3—Ni3 | 113.87 (11) |
C126—C125—H125 | 120.3 | C321—P3—Ni3 | 118.44 (11) |
C121—C126—C125 | 120.4 (3) | C312—C311—C316 | 118.7 (3) |
C121—C126—H126 | 119.8 | C312—C311—P3 | 121.1 (2) |
C125—C126—H126 | 119.8 | C316—C311—P3 | 119.6 (2) |
C132—C131—C136 | 118.0 (3) | C311—C312—C313 | 121.1 (3) |
C132—C131—P1 | 120.0 (3) | C311—C312—H312 | 119.4 |
C136—C131—P1 | 121.9 (3) | C313—C312—H312 | 119.4 |
C133—C132—C131 | 119.9 (3) | C314—C313—C312 | 119.7 (3) |
C133—C132—H132 | 120.1 | C314—C313—H313 | 120.1 |
C131—C132—H132 | 120.1 | C312—C313—H313 | 120.1 |
C134—C133—C132 | 121.1 (3) | C313—C314—C315 | 120.3 (3) |
C134—C133—H133 | 119.4 | C313—C314—H314 | 119.9 |
C132—C133—H133 | 119.4 | C315—C314—H314 | 119.9 |
C133—C134—C135 | 119.6 (3) | C314—C315—C316 | 120.1 (3) |
C133—C134—H134 | 120.2 | C314—C315—H315 | 120.0 |
C135—C134—H134 | 120.2 | C316—C315—H315 | 120.0 |
C136—C135—C134 | 119.8 (3) | C315—C316—C311 | 120.1 (3) |
C136—C135—H135 | 120.1 | C315—C316—H316 | 120.0 |
C134—C135—H135 | 120.1 | C311—C316—H316 | 120.0 |
C135—C136—C131 | 121.6 (3) | C322—C321—C326 | 118.7 (3) |
C135—C136—H136 | 119.2 | C322—C321—P3 | 119.9 (3) |
C131—C136—H136 | 119.2 | C326—C321—P3 | 121.4 (2) |
Cl2—Ni2—P2iii | 111.79 (3) | C321—C322—C323 | 119.9 (3) |
Cl2—Ni2—P2 | 111.79 (3) | C321—C322—H322 | 120.0 |
P2iii—Ni2—P2 | 107.06 (3) | C323—C322—H322 | 120.0 |
Cl2—Ni2—P2iv | 111.79 (3) | C324—C323—C322 | 120.8 (3) |
P2iii—Ni2—P2iv | 107.06 (3) | C324—C323—H323 | 119.6 |
P2—Ni2—P2iv | 107.06 (3) | C322—C323—H323 | 119.6 |
C211—P2—C231 | 106.07 (15) | C325—C324—C323 | 119.5 (3) |
C211—P2—C221 | 98.17 (15) | C325—C324—H324 | 120.2 |
C231—P2—C221 | 102.07 (15) | C323—C324—H324 | 120.2 |
C211—P2—Ni2 | 112.08 (11) | C324—C325—C326 | 120.4 (3) |
C231—P2—Ni2 | 115.89 (11) | C324—C325—H325 | 119.8 |
C221—P2—Ni2 | 120.31 (11) | C326—C325—H325 | 119.8 |
C212—C211—C216 | 118.9 (3) | C321—C326—C325 | 120.7 (3) |
C212—C211—P2 | 116.7 (2) | C321—C326—H326 | 119.7 |
C216—C211—P2 | 124.4 (3) | C325—C326—H326 | 119.7 |
C213—C212—C211 | 121.2 (3) | C336—C331—C332 | 118.5 (3) |
C213—C212—H212 | 119.4 | C336—C331—P3 | 116.6 (3) |
C211—C212—H212 | 119.4 | C332—C331—P3 | 124.8 (3) |
C212—C213—C214 | 119.2 (4) | C333—C332—C331 | 120.4 (4) |
C212—C213—H213 | 120.4 | C333—C332—H332 | 119.8 |
C214—C213—H213 | 120.4 | C331—C332—H332 | 119.8 |
C215—C214—C213 | 120.2 (4) | C332—C333—C334 | 120.5 (4) |
C215—C214—H214 | 119.9 | C332—C333—H333 | 119.7 |
C213—C214—H214 | 119.9 | C334—C333—H333 | 119.7 |
C214—C215—C216 | 120.5 (4) | C335—C334—C333 | 119.7 (4) |
C214—C215—H215 | 119.7 | C335—C334—H334 | 120.1 |
C216—C215—H215 | 119.7 | C333—C334—H334 | 120.1 |
C215—C216—C211 | 120.0 (3) | C334—C335—C336 | 119.8 (4) |
C215—C216—H216 | 120.0 | C334—C335—H335 | 120.1 |
C211—C216—H216 | 120.0 | C336—C335—H335 | 120.1 |
C222—C221—C226 | 118.7 (3) | C331—C336—C335 | 120.8 (4) |
C222—C221—P2 | 119.5 (2) | C331—C336—H336 | 119.6 |
C226—C221—P2 | 121.6 (2) | C335—C336—H336 | 119.6 |
| | | |
Cl1—Ni1—P1—C111 | −84.13 (11) | C211—P2—C221—C226 | −72.3 (3) |
P1i—Ni1—P1—C111 | 37.36 (12) | C231—P2—C221—C226 | 36.2 (3) |
P1ii—Ni1—P1—C111 | 154.39 (11) | Ni2—P2—C221—C226 | 166.1 (2) |
Cl1—Ni1—P1—C131 | 31.04 (12) | C226—C221—C222—C223 | −0.3 (5) |
P1i—Ni1—P1—C131 | 152.52 (12) | P2—C221—C222—C223 | −174.8 (3) |
P1ii—Ni1—P1—C131 | −90.45 (13) | C221—C222—C223—C224 | −0.5 (6) |
Cl1—Ni1—P1—C121 | 156.11 (12) | C222—C223—C224—C225 | 1.1 (6) |
P1i—Ni1—P1—C121 | −82.40 (12) | C223—C224—C225—C226 | −0.8 (6) |
P1ii—Ni1—P1—C121 | 34.63 (13) | C224—C225—C226—C221 | 0.0 (6) |
C131—P1—C111—C116 | −95.7 (3) | C222—C221—C226—C225 | 0.6 (5) |
C121—P1—C111—C116 | 158.6 (2) | P2—C221—C226—C225 | 175.0 (3) |
Ni1—P1—C111—C116 | 32.2 (3) | C211—P2—C231—C232 | 143.4 (3) |
C131—P1—C111—C112 | 82.4 (3) | C221—P2—C231—C232 | 41.1 (3) |
C121—P1—C111—C112 | −23.3 (3) | Ni2—P2—C231—C232 | −91.5 (3) |
Ni1—P1—C111—C112 | −149.7 (3) | C211—P2—C231—C236 | −44.6 (3) |
C116—C111—C112—C113 | −0.9 (5) | C221—P2—C231—C236 | −146.9 (3) |
P1—C111—C112—C113 | −178.9 (3) | Ni2—P2—C231—C236 | 80.5 (3) |
C111—C112—C113—C114 | −1.4 (6) | C236—C231—C232—C233 | 0.4 (5) |
C112—C113—C114—C115 | 2.0 (6) | P2—C231—C232—C233 | 172.6 (3) |
C113—C114—C115—C116 | −0.4 (5) | C231—C232—C233—C234 | −0.2 (5) |
C112—C111—C116—C115 | 2.5 (5) | C232—C233—C234—C235 | 0.0 (5) |
P1—C111—C116—C115 | −179.3 (3) | C233—C234—C235—C236 | 0.0 (5) |
C114—C115—C116—C111 | −1.9 (5) | C234—C235—C236—C231 | 0.3 (5) |
C111—P1—C121—C126 | 140.7 (3) | C232—C231—C236—C235 | −0.5 (5) |
C131—P1—C121—C126 | 37.6 (3) | P2—C231—C236—C235 | −172.5 (3) |
Ni1—P1—C121—C126 | −96.1 (3) | P3v—Ni3—P3—C311 | 85.85 (11) |
C111—P1—C121—C122 | −46.9 (3) | P3vi—Ni3—P3—C311 | −30.78 (12) |
C131—P1—C121—C122 | −150.0 (3) | Cl3—Ni3—P3—C311 | −152.47 (11) |
Ni1—P1—C121—C122 | 76.2 (3) | P3v—Ni3—P3—C331 | −35.95 (12) |
C126—C121—C122—C123 | 0.7 (5) | P3vi—Ni3—P3—C331 | −152.58 (11) |
P1—C121—C122—C123 | −171.7 (3) | Cl3—Ni3—P3—C331 | 85.74 (11) |
C121—C122—C123—C124 | −0.3 (5) | P3v—Ni3—P3—C321 | −150.96 (13) |
C122—C123—C124—C125 | −0.1 (6) | P3vi—Ni3—P3—C321 | 92.41 (14) |
C123—C124—C125—C126 | 0.1 (6) | Cl3—Ni3—P3—C321 | −29.27 (13) |
C122—C121—C126—C125 | −0.7 (5) | C331—P3—C311—C312 | −140.8 (3) |
P1—C121—C126—C125 | 171.7 (3) | C321—P3—C311—C312 | −38.0 (3) |
C124—C125—C126—C121 | 0.3 (6) | Ni3—P3—C311—C312 | 92.9 (3) |
C111—P1—C131—C132 | 111.3 (3) | C331—P3—C311—C316 | 48.0 (3) |
C121—P1—C131—C132 | −141.2 (3) | C321—P3—C311—C316 | 150.8 (3) |
Ni1—P1—C131—C132 | −10.0 (3) | Ni3—P3—C311—C316 | −78.4 (3) |
C111—P1—C131—C136 | −64.1 (3) | C316—C311—C312—C313 | 1.3 (5) |
C121—P1—C131—C136 | 43.4 (3) | P3—C311—C312—C313 | −170.0 (3) |
Ni1—P1—C131—C136 | 174.6 (2) | C311—C312—C313—C314 | −0.7 (5) |
C136—C131—C132—C133 | −2.7 (5) | C312—C313—C314—C315 | −0.5 (5) |
P1—C131—C132—C133 | −178.2 (3) | C313—C314—C315—C316 | 1.0 (5) |
C131—C132—C133—C134 | 1.8 (6) | C314—C315—C316—C311 | −0.3 (5) |
C132—C133—C134—C135 | −0.2 (6) | C312—C311—C316—C315 | −0.8 (5) |
C133—C134—C135—C136 | −0.4 (6) | P3—C311—C316—C315 | 170.6 (2) |
C134—C135—C136—C131 | −0.5 (6) | C311—P3—C321—C322 | 137.5 (3) |
C132—C131—C136—C135 | 2.0 (5) | C331—P3—C321—C322 | −114.6 (3) |
P1—C131—C136—C135 | 177.5 (3) | Ni3—P3—C321—C322 | 8.5 (3) |
Cl2—Ni2—P2—C211 | −82.58 (11) | C311—P3—C321—C326 | −46.0 (3) |
P2iii—Ni2—P2—C211 | 40.15 (12) | C331—P3—C321—C326 | 61.9 (3) |
P2iv—Ni2—P2—C211 | 154.69 (10) | Ni3—P3—C321—C326 | −175.0 (3) |
Cl2—Ni2—P2—C231 | 155.49 (12) | C326—C321—C322—C323 | −0.2 (6) |
P2iii—Ni2—P2—C231 | −81.77 (12) | P3—C321—C322—C323 | 176.4 (4) |
P2iv—Ni2—P2—C231 | 32.76 (13) | C321—C322—C323—C324 | −0.1 (8) |
Cl2—Ni2—P2—C221 | 31.92 (13) | C322—C323—C324—C325 | 0.3 (8) |
P2iii—Ni2—P2—C221 | 154.65 (13) | C323—C324—C325—C326 | 0.0 (7) |
P2iv—Ni2—P2—C221 | −90.81 (13) | C322—C321—C326—C325 | 0.5 (6) |
C231—P2—C211—C212 | 165.0 (2) | P3—C321—C326—C325 | −176.1 (3) |
C221—P2—C211—C212 | −89.9 (3) | C324—C325—C326—C321 | −0.3 (7) |
Ni2—P2—C211—C212 | 37.6 (3) | C311—P3—C331—C336 | −163.0 (3) |
C231—P2—C211—C216 | −18.1 (3) | C321—P3—C331—C336 | 90.6 (3) |
C221—P2—C211—C216 | 87.1 (3) | Ni3—P3—C331—C336 | −35.7 (3) |
Ni2—P2—C211—C216 | −145.5 (3) | C311—P3—C331—C332 | 19.5 (3) |
C216—C211—C212—C213 | −0.5 (5) | C321—P3—C331—C332 | −86.9 (3) |
P2—C211—C212—C213 | 176.6 (3) | Ni3—P3—C331—C332 | 146.8 (3) |
C211—C212—C213—C214 | 1.0 (6) | C336—C331—C332—C333 | 2.9 (5) |
C212—C213—C214—C215 | −1.1 (6) | P3—C331—C332—C333 | −179.6 (3) |
C213—C214—C215—C216 | 0.6 (6) | C331—C332—C333—C334 | 0.2 (6) |
C214—C215—C216—C211 | 0.0 (6) | C332—C333—C334—C335 | −3.1 (6) |
C212—C211—C216—C215 | 0.0 (5) | C333—C334—C335—C336 | 2.9 (6) |
P2—C211—C216—C215 | −176.9 (3) | C332—C331—C336—C335 | −3.1 (5) |
C211—P2—C221—C222 | 102.1 (3) | P3—C331—C336—C335 | 179.2 (3) |
C231—P2—C221—C222 | −149.4 (3) | C334—C335—C336—C331 | 0.3 (6) |
Ni2—P2—C221—C222 | −19.5 (3) | | |
Symmetry codes: (i) −x+y, −x, z; (ii) −y, x−y, z; (iii) −y+1, x−y+1, z; (iv) −x+y, −x+1, z; (v) −x+y+1, −x+1, z; (vi) −y+1, x−y, z. |