Chloro­bis­(tri­phenyl­phosphine)­nickel(I) tetra­hydro­furan solvate and an unsolvated trigonal phase of chloro­tris­(tri­phenyl­phosphine)­nickel(I)

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 Ni^I. A comparison is made between the form of [NiCl(PPh₃)₃] presented here and that of a known toluene solvate.

Computing details

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.

(I)

Crystal data

[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) Å^3	Plate, yellow
Z = 4	0.55 × 0.55 × 0.05 mm

Data collection

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

Refinement on F^2	Primary atom site location: heavy-atom method
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.096	H-atom parameters constrained
S = 1.02	w = 1/[σ^2(Fo^2) + (0.0469P)^2 + 2.2443P] where P = (Fo^2 + 2Fc^2)/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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

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)

(II)

Crystal data

[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) Å^3	T = 150 K
Z = 3	Block, yellow
F(000) = 1377	0.50 × 0.25 × 0.25 mm

Data collection

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

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.031	H-atom parameters constrained
wR(F^2) = 0.066	w = 1/[σ^2(Fo^2) + (0.026P)^2 + 0.0482P] where P = (Fo^2 + 2Fc^2)/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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Ni1—Cl1	2.2933 (17)	C222—C223	1.392 (5)
Ni1—P1^i	2.3082 (9)	C222—H222	0.9500
Ni1—P1	2.3082 (9)	C223—C224	1.369 (6)
Ni1—P1^ii	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—P3^v	2.2966 (9)
C122—H122	0.9500	Ni3—P3^vi	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—P2^iii	2.2887 (9)	C322—H322	0.9500
Ni2—P2	2.2887 (9)	C323—C324	1.379 (5)
Ni2—P2^iv	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—P1^i	110.71 (3)	C221—C222—C223	119.9 (3)
Cl1—Ni1—P1	110.71 (3)	C221—C222—H222	120.1
P1^i—Ni1—P1	108.21 (3)	C223—C222—H222	120.1
Cl1—Ni1—P1^ii	110.71 (3)	C224—C223—C222	121.0 (3)
P1^i—Ni1—P1^ii	108.21 (3)	C224—C223—H223	119.5
P1—Ni1—P1^ii	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)	P3^v—Ni3—P3^vi	108.03 (3)
C123—C122—H122	120.1	P3^v—Ni3—P3	108.03 (3)
C121—C122—H122	120.1	P3^vi—Ni3—P3	108.03 (3)
C124—C123—C122	120.4 (3)	P3^v—Ni3—Cl3	110.88 (3)
C124—C123—H123	119.8	P3^vi—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—P2^iii	111.79 (3)	C321—C322—C323	119.9 (3)
Cl2—Ni2—P2	111.79 (3)	C321—C322—H322	120.0
P2^iii—Ni2—P2	107.06 (3)	C323—C322—H322	120.0
Cl2—Ni2—P2^iv	111.79 (3)	C324—C323—C322	120.8 (3)
P2^iii—Ni2—P2^iv	107.06 (3)	C324—C323—H323	119.6
P2—Ni2—P2^iv	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)
P1^i—Ni1—P1—C111	37.36 (12)	C231—P2—C221—C226	36.2 (3)
P1^ii—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)
P1^i—Ni1—P1—C131	152.52 (12)	P2—C221—C222—C223	−174.8 (3)
P1^ii—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)
P1^i—Ni1—P1—C121	−82.40 (12)	C223—C224—C225—C226	−0.8 (6)
P1^ii—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)	P3^v—Ni3—P3—C311	85.85 (11)
C111—P1—C121—C122	−46.9 (3)	P3^vi—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)	P3^v—Ni3—P3—C331	−35.95 (12)
C126—C121—C122—C123	0.7 (5)	P3^vi—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)	P3^v—Ni3—P3—C321	−150.96 (13)
C122—C123—C124—C125	−0.1 (6)	P3^vi—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)
P2^iii—Ni2—P2—C211	40.15 (12)	C331—P3—C321—C326	61.9 (3)
P2^iv—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)
P2^iii—Ni2—P2—C231	−81.77 (12)	P3—C321—C322—C323	176.4 (4)
P2^iv—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)
P2^iii—Ni2—P2—C221	154.65 (13)	C323—C324—C325—C326	0.0 (7)
P2^iv—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.