Tris(tri-o-tolyl phosphite-κP)nickel: a coordinatively unsaturated nickel(0) complex

A previously reported complex, [Ni(C₂₁H₂₁O₃P)₃] or Ni[P(O-o-tolyl₃)₃] [Gosser & Tolman (1970). Inorg. Chem. 9, 2350–2353], crystallized in the monoclinic space group C2/c, and its solid-state structure was determined. The Ni⁰ atom adopts an essentially trigonal-planar geometry as a consequence of the steric congestion of the ligands. Three of the phenoxy rings on two phosphite ligands were modelled as being disordered over two sets of sites, and the occupancy factors were set at 0.5 after trial refinement and intramolecular contact considerations. The exact ligand cone angle has been calculated to be 163.6°.

S1. Experimental

S1.1. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 1. Two of the phen­oxy rings on P2 and one on P1 were all modelled as being disordered over two sets of sites. Occupancy factors were set at 0.5 after trial refinement and intra­molecular contact considerations. Geometries of the disordered components were restrained to ideal values with the atoms refined with isotropic displacement parameters after anisotropic refinement resulted in unacceptable ellipsoids even with reasonable restraints. There was no indication that the disorder resulted from a 2-fold rotation of the o-tolyl groups about the C—O bonds.

S2. Results and discussion

Computing details

Data collection: CrysAlis PRO (Agilent, 2013); cell refinement: CrysAlis PRO (Agilent, 2013); data reduction: CrysAlis PRO (Agilent, 2013); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 2012).

Figures

Fig. 1. The structure of the molecule of (I), projected onto the plane of the P atoms, showing the atom-numbering scheme. Displacement ellipsoids are drawn at the ??% probability level. [Please complete] Only one of each of the disordered groups is shown. H atoms have been omitted. []

Tris(tri-o-tolylphosphite-κP)nickel(II)

Crystal data

[Ni(C21H21O3P)3]	F(000) = 4688
Mr = 1115.75	Dx = 1.323 Mg m^−3
Monoclinic, C2/c	Cu Kα radiation, λ = 1.54178 Å
Hall symbol: -C 2yc	Cell parameters from 15074 reflections
a = 21.5898 (9) Å	θ = 4.1–67.1°
b = 12.3292 (3) Å	µ = 1.77 mm^−1
c = 43.403 (2) Å	T = 100 K
β = 104.129 (5)°	Needle, orange
V = 11203.8 (7) Å^3	0.28 × 0.11 × 0.07 mm
Z = 8

Data collection

Oxford Gemini diffractometer	9993 independent reflections
Radiation source: sealed X-ray tube	8185 reflections with I > 2σ(I)
Mirror monochromator	Rint = 0.043
Detector resolution: 10.4738 pixels mm^-1	θmax = 67.4°, θmin = 4.2°
ω scans	h = −25→25
Absorption correction: analytical (CrysAlis PRO; Agilent, 2013)	k = −14→9
Tmin = 0.726, Tmax = 0.896	l = −51→51
56232 measured reflections

Refinement

Refinement on F^2	82 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.099	H-atom parameters constrained
wR(F^2) = 0.259	w = 1/[σ^2(Fo^2) + (0.1046P)^2 + 70.9791P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.003
9993 reflections	Δρmax = 1.26 e Å^−3
682 parameters	Δρmin = −1.41 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Ni1	0.16191 (5)	0.01350 (7)	0.13447 (2)	0.0662 (3)
P1	0.12143 (6)	0.07529 (12)	0.08885 (3)	0.0554 (4)
O11	0.1535 (4)	0.0437 (7)	0.06232 (18)	0.0509 (19)*	0.5
C111	0.1564 (5)	−0.0534 (10)	0.0461 (2)	0.051 (2)*	0.5
C112	0.1878 (7)	−0.0500 (11)	0.0224 (3)	0.087 (4)*	0.5
C113	0.1882 (9)	−0.1420 (14)	0.0031 (4)	0.106 (6)*	0.5
H113	0.205	−0.1397	−0.0152	0.127*	0.5
C114	0.1626 (8)	−0.2364 (12)	0.0126 (4)	0.107 (5)*	0.5
H114	0.1676	−0.3019	0.0019	0.128*	0.5
C115	0.1305 (7)	−0.2413 (10)	0.0363 (3)	0.088 (4)*	0.5
H115	0.112	−0.3073	0.0411	0.106*	0.5
C116	0.1260 (5)	−0.1466 (8)	0.0532 (2)	0.057 (3)*	0.5
H116	0.1027	−0.1457	0.0692	0.068*	0.5
C117	0.2158 (8)	0.0607 (14)	0.0139 (4)	0.084 (4)*	0.5
H11A	0.2501	0.0843	0.0319	0.126*	0.5
H11B	0.1819	0.1155	0.0095	0.126*	0.5
H11C	0.2328	0.0511	−0.0049	0.126*	0.5
O41	0.1572 (3)	0.0836 (7)	0.05713 (18)	0.0484 (18)*	0.5
C141	0.1642 (5)	−0.0077 (8)	0.0398 (2)	0.049 (2)*	0.5
C142	0.1933 (6)	0.0071 (9)	0.0154 (3)	0.060 (3)*	0.5
C143	0.1994 (6)	−0.0788 (10)	−0.0042 (3)	0.077 (3)*	0.5
H143	0.2155	−0.068	−0.0225	0.093*	0.5
C144	0.1807 (6)	−0.1844 (10)	0.0039 (3)	0.064 (3)*	0.5
H144	0.1894	−0.2457	−0.0076	0.077*	0.5
C145	0.1514 (6)	−0.1982 (9)	0.0273 (3)	0.074 (3)*	0.5
H145	0.1342	−0.2669	0.0306	0.089*	0.5
C146	0.1462 (5)	−0.1107 (9)	0.0468 (2)	0.048 (2)*	0.5
H146	0.1301	−0.1219	0.065	0.058*	0.5
C147	0.2130 (7)	0.1270 (12)	0.0085 (3)	0.074 (3)*	0.5
H14A	0.2495	0.1502	0.0255	0.112*	0.5
H14B	0.1769	0.176	0.0078	0.112*	0.5
H14C	0.2248	0.129	−0.0119	0.112*	0.5
O12	0.05100 (16)	0.0424 (3)	0.06782 (8)	0.0545 (8)
C121	−0.0027 (3)	0.0245 (5)	0.07937 (13)	0.0577 (13)
C122	−0.0489 (3)	−0.0423 (6)	0.06046 (15)	0.0792 (19)
C123	−0.1043 (4)	−0.0602 (9)	0.0711 (2)	0.123 (4)
H123	−0.137	−0.1049	0.0589	0.147*
C124	−0.1126 (4)	−0.0151 (9)	0.0987 (2)	0.121 (4)
H124	−0.1508	−0.0287	0.1053	0.145*
C125	−0.0658 (4)	0.0495 (8)	0.11691 (17)	0.096 (2)
H125	−0.0712	0.0794	0.1363	0.116*
C126	−0.0104 (3)	0.0712 (5)	0.10677 (13)	0.0658 (14)
H126	0.0216	0.1179	0.1188	0.079*
C127	−0.0392 (4)	−0.0932 (8)	0.03009 (18)	0.104 (3)
H12A	−0.0709	−0.1505	0.0231	0.156*
H12B	0.0038	−0.1243	0.0341	0.156*
H12C	−0.0442	−0.0376	0.0135	0.156*
O13	0.11931 (18)	0.2075 (3)	0.08807 (8)	0.0590 (9)
C131	0.0991 (3)	0.2709 (5)	0.06014 (14)	0.0659 (15)
C132	0.1439 (4)	0.3287 (7)	0.04999 (17)	0.092 (2)
C133	0.1223 (5)	0.3921 (8)	0.0223 (2)	0.109 (3)
H133	0.1524	0.432	0.0142	0.131*
C134	0.0592 (4)	0.3971 (7)	0.00709 (18)	0.093 (2)
H134	0.0459	0.4399	−0.0116	0.112*
C135	0.0153 (4)	0.3415 (6)	0.01838 (16)	0.0831 (19)
H135	−0.0287	0.3466	0.0079	0.1*
C136	0.0345 (3)	0.2771 (5)	0.04520 (14)	0.0673 (15)
H136	0.004	0.2378	0.0532	0.081*
C137	0.2125 (4)	0.3238 (10)	0.0674 (2)	0.133 (4)
H13A	0.2159	0.3237	0.0903	0.2*
H13B	0.235	0.3872	0.0618	0.2*
H13C	0.2318	0.2575	0.0615	0.2*
P2	0.2204 (3)	−0.1216 (6)	0.14246 (17)	0.0443 (11)	0.5
P2'	0.2379 (3)	−0.1055 (6)	0.13774 (18)	0.0539 (14)	0.5
O21	0.27639 (15)	−0.1313 (3)	0.17414 (8)	0.0475 (7)
C211	0.3215 (2)	−0.2155 (4)	0.18260 (11)	0.0489 (11)
C212	0.3076 (3)	−0.3061 (4)	0.19741 (14)	0.0616 (14)
C213	0.3563 (4)	−0.3821 (5)	0.20770 (15)	0.080 (2)
H213	0.3472	−0.4466	0.2177	0.096*
C214	0.4154 (4)	−0.3670 (7)	0.20392 (17)	0.092 (2)
H214	0.4478	−0.4196	0.2113	0.11*
C215	0.4285 (3)	−0.2741 (8)	0.1892 (2)	0.102 (3)
H215	0.4704	−0.2623	0.1865	0.122*
C216	0.3818 (3)	−0.1985 (5)	0.17827 (16)	0.0709 (16)
H216	0.3909	−0.1349	0.1678	0.085*
C217	0.2442 (4)	−0.3264 (6)	0.2043 (2)	0.106 (3)
H21A	0.2217	−0.2574	0.2042	0.16*
H21B	0.2504	−0.3609	0.2251	0.16*
H21C	0.2189	−0.3743	0.1879	0.16*
O22	0.1922 (3)	−0.2400 (5)	0.14174 (14)	0.0385 (12)*	0.5
C221	0.1277 (4)	−0.2482 (8)	0.1297 (3)	0.058 (3)*	0.5
C222	0.1058 (5)	−0.3344 (9)	0.1094 (3)	0.066 (3)*	0.5
C223	0.0385 (6)	−0.3432 (12)	0.1008 (4)	0.092 (5)*	0.5
H223	0.0206	−0.4059	0.0893	0.11*	0.5
C224	−0.0016 (7)	−0.2705 (14)	0.1075 (5)	0.118 (6)*	0.5
H224	−0.0462	−0.2767	0.0986	0.141*	0.5
C225	0.0227 (6)	−0.1847 (11)	0.1280 (3)	0.090 (4)*	0.5
H225	−0.0053	−0.1345	0.1342	0.109*	0.5
C226	0.0863 (5)	−0.1744 (9)	0.1387 (3)	0.068 (3)*	0.5
H226	0.1033	−0.1163	0.1526	0.081*	0.5
C227	0.1518 (8)	−0.4181 (15)	0.1029 (4)	0.096 (4)*	0.5
H22A	0.1616	−0.4704	0.1204	0.144*	0.5
H22B	0.1912	−0.3823	0.101	0.144*	0.5
H22C	0.1324	−0.456	0.083	0.144*	0.5
O24	0.2143 (6)	−0.2238 (11)	0.1255 (3)	0.125 (4)*	0.5
C241	0.1500 (7)	−0.2572 (14)	0.1163 (4)	0.111 (5)*	0.5
C242	0.1501 (7)	−0.3444 (17)	0.0954 (5)	0.118 (6)*	0.5
C243	0.0904 (9)	−0.3860 (18)	0.0793 (5)	0.156 (9)*	0.5
H243	0.0872	−0.4421	0.064	0.187*	0.5
C244	0.0398 (7)	−0.3458 (14)	0.0858 (4)	0.100 (5)*	0.5
H244	0.0002	−0.3747	0.0742	0.12*	0.5
C245	0.0364 (10)	−0.264 (3)	0.1081 (8)	0.227 (16)*	0.5
H245	−0.003	−0.2416	0.112	0.273*	0.5
C246	0.0955 (11)	−0.219 (2)	0.1241 (6)	0.180 (12)*	0.5
H246	0.0978	−0.1645	0.1398	0.216*	0.5
C247	0.1950 (12)	−0.394 (2)	0.0864 (6)	0.154 (9)*	0.5
H24A	0.1763	−0.4443	0.0691	0.232*	0.5
H24B	0.2211	−0.4351	0.1043	0.232*	0.5
H24C	0.2219	−0.3413	0.0789	0.232*	0.5
O23	0.2619 (3)	−0.1528 (6)	0.11591 (15)	0.0488 (15)*	0.5
C231	0.3002 (7)	−0.0896 (11)	0.1033 (4)	0.080 (4)*	0.5
C232	0.3354 (9)	−0.1481 (13)	0.0852 (5)	0.113 (6)*	0.5
C233	0.3770 (10)	−0.0839 (16)	0.0731 (5)	0.144 (8)*	0.5
H233	0.4045	−0.1185	0.0621	0.173*	0.5
C234	0.3803 (11)	0.0244 (16)	0.0763 (6)	0.146 (9)*	0.5
H234	0.4057	0.0644	0.0653	0.176*	0.5
C235	0.3467 (10)	0.0811 (13)	0.0958 (5)	0.128 (7)*	0.5
H235	0.3506	0.1572	0.0991	0.153*	0.5
C236	0.3078 (7)	0.0170 (12)	0.1095 (3)	0.076 (4)*	0.5
H236	0.2859	0.0495	0.1237	0.091*	0.5
C237	0.3240 (11)	−0.2742 (18)	0.0817 (6)	0.134 (7)*	0.5
H23A	0.357	−0.307	0.0727	0.201*	0.5
H23B	0.2818	−0.2882	0.0676	0.201*	0.5
H23C	0.326	−0.3059	0.1026	0.201*	0.5
O25	0.2926 (6)	−0.1144 (10)	0.1198 (3)	0.104 (3)*	0.5
C251	0.3143 (5)	−0.0379 (8)	0.1035 (2)	0.048 (2)*	0.5
C252	0.3404 (5)	−0.0829 (7)	0.0801 (2)	0.050 (2)*	0.5
C253	0.3678 (6)	−0.0120 (9)	0.0623 (3)	0.070 (3)*	0.5
H253	0.3866	−0.0391	0.0463	0.084*	0.5
C254	0.3674 (6)	0.0983 (9)	0.0681 (3)	0.078 (3)*	0.5
H254	0.3863	0.1464	0.056	0.094*	0.5
C255	0.3396 (6)	0.1405 (10)	0.0916 (3)	0.075 (3)*	0.5
H255	0.3404	0.2164	0.0956	0.09*	0.5
C256	0.3111 (6)	0.0713 (9)	0.1089 (3)	0.066 (3)*	0.5
H256	0.2899	0.0982	0.1241	0.079*	0.5
C257	0.3424 (7)	−0.2038 (12)	0.0751 (3)	0.074 (3)*	0.5
H25A	0.3785	−0.2218	0.0661	0.112*	0.5
H25B	0.3025	−0.2273	0.0605	0.112*	0.5
H25C	0.3474	−0.241	0.0955	0.112*	0.5
P3	0.16286 (6)	0.12118 (9)	0.17181 (3)	0.0470 (3)
O31	0.21613 (16)	0.2161 (3)	0.18060 (9)	0.0544 (8)
C311	0.2803 (2)	0.2064 (4)	0.18050 (12)	0.0515 (11)
C312	0.3070 (3)	0.2956 (4)	0.16922 (15)	0.0647 (14)
C313	0.3713 (3)	0.2905 (5)	0.16969 (19)	0.082 (2)
H313	0.3908	0.3505	0.1621	0.099*
C314	0.4079 (3)	0.1999 (5)	0.18096 (18)	0.0797 (19)
H314	0.4516	0.1973	0.1805	0.096*
C315	0.3803 (3)	0.1134 (4)	0.19291 (15)	0.0646 (15)
H315	0.4054	0.0518	0.2012	0.077*
C316	0.3161 (3)	0.1166 (4)	0.19284 (13)	0.0551 (12)
H316	0.2969	0.0577	0.2012	0.066*
C317	0.2669 (3)	0.3949 (5)	0.15789 (18)	0.0779 (18)
H31A	0.2322	0.3757	0.1395	0.117*
H31B	0.2936	0.4512	0.1518	0.117*
H31C	0.2487	0.422	0.175	0.117*
O32	0.17334 (16)	0.0753 (3)	0.20817 (8)	0.0542 (8)
C321	0.1375 (3)	−0.0127 (4)	0.21457 (14)	0.0587 (13)
C322	0.1707 (3)	−0.0944 (4)	0.23422 (13)	0.0611 (14)
C323	0.1337 (4)	−0.1801 (5)	0.24155 (17)	0.078 (2)
H323	0.1544	−0.2368	0.255	0.094*
C324	0.0686 (4)	−0.1845 (5)	0.2298 (2)	0.095 (3)
H324	0.0452	−0.2443	0.2349	0.114*
C325	0.0379 (4)	−0.1031 (6)	0.2111 (2)	0.100 (3)
H325	−0.0072	−0.1057	0.2031	0.12*
C326	0.0725 (3)	−0.0160 (5)	0.20359 (19)	0.0785 (19)
H326	0.0509	0.0414	0.1908	0.094*
C327	0.2406 (3)	−0.0898 (5)	0.24717 (13)	0.0674 (15)
H32A	0.2621	−0.1034	0.2301	0.101*
H32B	0.2535	−0.145	0.2637	0.101*
H32C	0.2526	−0.0178	0.2563	0.101*
O33	0.10088 (16)	0.1985 (2)	0.16775 (7)	0.0484 (8)
C331	0.0935 (2)	0.2915 (4)	0.18534 (12)	0.0470 (11)
C332	0.0728 (4)	0.3820 (5)	0.16820 (15)	0.084 (2)
C333	0.0619 (5)	0.4740 (6)	0.18498 (18)	0.109 (3)
H333	0.0476	0.5386	0.1735	0.13*
C334	0.0710 (4)	0.4743 (6)	0.21727 (17)	0.084 (2)
H334	0.0641	0.5384	0.2281	0.101*
C335	0.0903 (3)	0.3808 (6)	0.23366 (14)	0.0765 (19)
H335	0.0959	0.3789	0.2561	0.092*
C336	0.1017 (3)	0.2887 (5)	0.21771 (12)	0.0593 (13)
H336	0.1151	0.2237	0.2291	0.071*
C337	0.0616 (6)	0.3832 (7)	0.13258 (18)	0.144 (4)
H33A	0.0919	0.3341	0.1262	0.216*
H33B	0.0677	0.457	0.1255	0.216*
H33C	0.0178	0.3594	0.1229	0.216*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0747 (6)	0.0502 (5)	0.0595 (6)	0.0233 (4)	−0.0109 (5)	−0.0147 (4)
P1	0.0483 (7)	0.0599 (8)	0.0532 (7)	0.0110 (6)	0.0029 (6)	−0.0140 (6)
O12	0.053 (2)	0.055 (2)	0.0511 (19)	0.0028 (16)	0.0041 (15)	−0.0056 (15)
C121	0.056 (3)	0.063 (3)	0.052 (3)	−0.010 (2)	0.009 (2)	0.004 (2)
C122	0.075 (4)	0.096 (5)	0.062 (4)	−0.028 (4)	0.009 (3)	−0.013 (3)
C123	0.114 (7)	0.173 (9)	0.082 (5)	−0.081 (7)	0.025 (5)	−0.024 (6)
C124	0.099 (6)	0.185 (10)	0.081 (5)	−0.070 (6)	0.027 (4)	−0.012 (6)
C125	0.093 (5)	0.139 (7)	0.061 (4)	−0.035 (5)	0.027 (4)	−0.007 (4)
C126	0.064 (3)	0.074 (4)	0.056 (3)	−0.006 (3)	0.008 (3)	−0.004 (3)
C127	0.084 (5)	0.134 (7)	0.083 (5)	−0.031 (5)	0.002 (4)	−0.042 (5)
O13	0.067 (2)	0.060 (2)	0.0487 (19)	−0.0053 (17)	0.0107 (16)	−0.0033 (16)
C131	0.084 (4)	0.059 (3)	0.057 (3)	−0.009 (3)	0.022 (3)	−0.005 (3)
C132	0.088 (5)	0.111 (6)	0.073 (4)	−0.034 (4)	0.014 (4)	0.001 (4)
C133	0.113 (7)	0.124 (7)	0.089 (5)	−0.032 (5)	0.024 (5)	0.022 (5)
C134	0.111 (6)	0.098 (6)	0.071 (4)	−0.014 (5)	0.023 (4)	0.008 (4)
C135	0.095 (5)	0.074 (4)	0.075 (4)	0.004 (4)	0.012 (4)	0.009 (3)
C136	0.081 (4)	0.058 (3)	0.063 (3)	0.006 (3)	0.018 (3)	0.003 (3)
C137	0.091 (6)	0.185 (11)	0.117 (7)	−0.055 (7)	0.013 (5)	0.023 (7)
P2	0.041 (3)	0.048 (2)	0.044 (2)	0.0034 (17)	0.0107 (16)	−0.0104 (16)
P2'	0.058 (4)	0.045 (3)	0.055 (3)	0.018 (2)	0.007 (2)	−0.0050 (18)
O21	0.0491 (18)	0.0452 (18)	0.0496 (18)	0.0076 (14)	0.0144 (14)	0.0005 (14)
C211	0.046 (3)	0.052 (3)	0.047 (3)	0.010 (2)	0.009 (2)	−0.003 (2)
C212	0.072 (4)	0.053 (3)	0.067 (3)	0.018 (3)	0.031 (3)	0.005 (3)
C213	0.112 (6)	0.073 (4)	0.060 (3)	0.044 (4)	0.030 (3)	0.014 (3)
C214	0.080 (5)	0.107 (6)	0.076 (4)	0.049 (4)	−0.005 (4)	−0.015 (4)
C215	0.042 (3)	0.125 (7)	0.130 (7)	0.016 (4)	0.005 (4)	−0.040 (6)
C216	0.047 (3)	0.077 (4)	0.086 (4)	−0.001 (3)	0.012 (3)	−0.014 (3)
C217	0.109 (6)	0.057 (4)	0.184 (9)	0.018 (4)	0.096 (6)	0.023 (5)
P3	0.0531 (7)	0.0338 (6)	0.0487 (7)	0.0011 (5)	0.0022 (5)	0.0010 (5)
O31	0.057 (2)	0.0375 (17)	0.068 (2)	−0.0029 (15)	0.0149 (17)	−0.0048 (15)
C311	0.053 (3)	0.043 (3)	0.057 (3)	−0.004 (2)	0.010 (2)	−0.004 (2)
C312	0.070 (4)	0.047 (3)	0.077 (4)	0.005 (3)	0.019 (3)	0.012 (3)
C313	0.064 (4)	0.062 (4)	0.128 (6)	−0.003 (3)	0.036 (4)	0.021 (4)
C314	0.061 (4)	0.061 (4)	0.119 (6)	0.001 (3)	0.026 (4)	0.010 (4)
C315	0.056 (3)	0.046 (3)	0.086 (4)	−0.001 (2)	0.005 (3)	−0.003 (3)
C316	0.060 (3)	0.036 (2)	0.067 (3)	−0.006 (2)	0.011 (2)	−0.004 (2)
C317	0.081 (4)	0.056 (3)	0.101 (5)	0.005 (3)	0.030 (4)	0.023 (3)
O32	0.058 (2)	0.0459 (18)	0.0530 (19)	0.0013 (15)	0.0024 (15)	0.0090 (15)
C321	0.065 (3)	0.045 (3)	0.070 (3)	0.008 (2)	0.023 (3)	0.015 (2)
C322	0.079 (4)	0.053 (3)	0.060 (3)	0.023 (3)	0.033 (3)	0.014 (2)
C323	0.104 (5)	0.052 (3)	0.097 (5)	0.028 (3)	0.059 (4)	0.030 (3)
C324	0.096 (5)	0.060 (4)	0.155 (7)	0.016 (4)	0.081 (5)	0.033 (4)
C325	0.074 (4)	0.062 (4)	0.175 (8)	0.011 (3)	0.053 (5)	0.029 (5)
C326	0.065 (4)	0.049 (3)	0.125 (6)	0.010 (3)	0.030 (4)	0.025 (3)
C327	0.085 (4)	0.065 (3)	0.050 (3)	0.026 (3)	0.012 (3)	0.014 (3)
O33	0.0554 (19)	0.0374 (17)	0.0475 (17)	0.0032 (14)	0.0032 (14)	−0.0003 (13)
C331	0.046 (3)	0.041 (2)	0.054 (3)	−0.0001 (19)	0.012 (2)	−0.002 (2)
C332	0.152 (7)	0.048 (3)	0.057 (3)	0.026 (4)	0.038 (4)	0.005 (3)
C333	0.201 (10)	0.051 (4)	0.080 (5)	0.041 (5)	0.047 (5)	0.000 (3)
C334	0.101 (5)	0.075 (4)	0.076 (4)	0.025 (4)	0.021 (4)	−0.023 (3)
C335	0.068 (4)	0.106 (5)	0.053 (3)	0.030 (4)	0.010 (3)	−0.012 (3)
C336	0.056 (3)	0.070 (3)	0.049 (3)	0.014 (3)	0.007 (2)	0.003 (2)
C337	0.283 (12)	0.084 (5)	0.069 (4)	0.093 (7)	0.051 (6)	0.021 (4)

Geometric parameters (Å, º)

Ni1—P2	2.068 (8)	C225—H225	0.95
Ni1—P3	2.0915 (15)	C226—H226	0.95
Ni1—P1	2.1021 (17)	C227—H22A	0.98
Ni1—P2'	2.179 (7)	C227—H22B	0.98
P1—O11	1.531 (8)	C227—H22C	0.98
P1—O12	1.622 (4)	O24—C241	1.409 (14)
P1—O13	1.631 (4)	C241—C246	1.382 (15)
P1—O41	1.738 (8)	C241—C242	1.407 (15)
O11—C111	1.397 (13)	C242—C247	1.29 (3)
C111—C112	1.368 (13)	C242—C243	1.406 (15)
C111—C116	1.394 (12)	C243—C244	1.291 (15)
C112—C113	1.411 (14)	C243—H243	0.95
C112—C117	1.57 (2)	C244—C245	1.406 (16)
C113—C114	1.394 (15)	C244—H244	0.95
C113—H113	0.95	C245—C246	1.412 (16)
C114—C115	1.378 (14)	C245—H245	0.95
C114—H114	0.95	C246—H246	0.95
C115—C116	1.395 (13)	C247—H24A	0.98
C115—H115	0.95	C247—H24B	0.98
C116—H116	0.95	C247—H24C	0.98
C117—H11A	0.98	O23—C231	1.345 (13)
C117—H11B	0.98	C231—C236	1.344 (14)
C117—H11C	0.98	C231—C232	1.418 (14)
O41—C141	1.382 (11)	C232—C233	1.392 (15)
C141—C142	1.371 (12)	C232—C237	1.58 (3)
C141—C146	1.382 (12)	C233—C234	1.343 (15)
C142—C143	1.386 (12)	C233—H233	0.95
C142—C147	1.586 (17)	C234—C235	1.424 (15)
C143—C144	1.432 (13)	C234—H234	0.95
C143—H143	0.95	C235—C236	1.388 (14)
C144—C145	1.332 (13)	C235—H235	0.95
C144—H144	0.95	C236—H236	0.95
C145—C146	1.393 (12)	C237—H23A	0.98
C145—H145	0.95	C237—H23B	0.98
C146—H146	0.95	C237—H23C	0.98
C147—H14A	0.98	O25—C251	1.333 (13)
C147—H14B	0.98	C251—C256	1.371 (12)
C147—H14C	0.98	C251—C252	1.392 (11)
O12—C121	1.388 (6)	C252—C253	1.388 (12)
C121—C126	1.368 (8)	C252—C257	1.508 (17)
C121—C122	1.395 (8)	C253—C254	1.383 (13)
C122—C123	1.401 (10)	C253—H253	0.95
C122—C127	1.520 (10)	C254—C255	1.405 (13)
C123—C124	1.372 (12)	C254—H254	0.95
C123—H123	0.95	C255—C256	1.376 (13)
C124—C125	1.375 (11)	C255—H255	0.95
C124—H124	0.95	C256—H256	0.95
C125—C126	1.399 (9)	C257—H25A	0.98
C125—H125	0.95	C257—H25B	0.98
C126—H126	0.95	C257—H25C	0.98
C127—H12A	0.98	P3—O33	1.617 (3)
C127—H12B	0.98	P3—O31	1.620 (3)
C127—H12C	0.98	P3—O32	1.639 (3)
O13—C131	1.418 (7)	O31—C311	1.393 (6)
C131—C132	1.358 (9)	C311—C316	1.381 (7)
C131—C136	1.389 (9)	C311—C312	1.385 (7)
C132—C133	1.413 (11)	C312—C313	1.383 (8)
C132—C137	1.492 (11)	C312—C317	1.511 (8)
C133—C134	1.363 (12)	C313—C314	1.386 (9)
C133—H133	0.95	C313—H313	0.95
C134—C135	1.355 (10)	C314—C315	1.382 (8)
C134—H134	0.95	C314—H314	0.95
C135—C136	1.387 (9)	C315—C316	1.386 (8)
C135—H135	0.95	C315—H315	0.95
C136—H136	0.95	C316—H316	0.95
C137—H13A	0.98	C317—H31A	0.98
C137—H13B	0.98	C317—H31B	0.98
C137—H13C	0.98	C317—H31C	0.98
P2—O22	1.579 (9)	O32—C321	1.399 (6)
P2—O21	1.599 (8)	C321—C326	1.369 (9)
P2—O23	1.668 (8)	C321—C322	1.398 (7)
P2'—O25	1.568 (14)	C322—C323	1.406 (8)
P2'—O24	1.593 (15)	C322—C327	1.478 (9)
P2'—O21	1.627 (9)	C323—C324	1.373 (11)
O21—C211	1.408 (5)	C323—H323	0.95
C211—C212	1.358 (7)	C324—C325	1.359 (10)
C211—C216	1.376 (8)	C324—H324	0.95
C212—C213	1.398 (8)	C325—C326	1.392 (9)
C212—C217	1.491 (8)	C325—H325	0.95
C213—C214	1.339 (11)	C326—H326	0.95
C213—H213	0.95	C327—H32A	0.98
C214—C215	1.374 (12)	C327—H32B	0.98
C214—H214	0.95	C327—H32C	0.98
C215—C216	1.372 (10)	O33—C331	1.407 (6)
C215—H215	0.95	C331—C332	1.355 (7)
C216—H216	0.95	C331—C336	1.373 (7)
C217—H21A	0.98	C332—C333	1.400 (8)
C217—H21B	0.98	C332—C337	1.505 (9)
C217—H21C	0.98	C333—C334	1.366 (10)
O22—C221	1.367 (10)	C333—H333	0.95
C221—C222	1.387 (12)	C334—C335	1.366 (10)
C221—C226	1.396 (13)	C334—H334	0.95
C222—C223	1.413 (13)	C335—C336	1.382 (8)
C222—C227	1.505 (19)	C335—H335	0.95
C223—C224	1.328 (14)	C336—H336	0.95
C223—H223	0.95	C337—H33A	0.98
C224—C225	1.397 (14)	C337—H33B	0.98
C224—H224	0.95	C337—H33C	0.98
C225—C226	1.345 (13)
P2—Ni1—P3	119.4 (2)	C224—C225—H225	120.5
P2—Ni1—P1	123.1 (2)	C225—C226—C221	120.6 (10)
P3—Ni1—P1	115.03 (6)	C225—C226—H226	119.7
P3—Ni1—P2'	120.8 (2)	C221—C226—H226	119.7
P1—Ni1—P2'	116.0 (2)	C222—C227—H22A	109.5
O11—P1—O12	92.7 (3)	C222—C227—H22B	109.5
O11—P1—O13	104.7 (4)	H22A—C227—H22B	109.5
O12—P1—O13	102.74 (19)	C222—C227—H22C	109.5
O12—P1—O41	96.1 (3)	H22A—C227—H22C	109.5
O13—P1—O41	86.6 (3)	H22B—C227—H22C	109.5
O11—P1—Ni1	117.1 (3)	C241—O24—P2'	125.1 (12)
O12—P1—Ni1	123.80 (16)	C246—C241—C242	123.5 (12)
O13—P1—Ni1	112.65 (14)	C246—C241—O24	132.1 (16)
O41—P1—Ni1	127.2 (3)	C242—C241—O24	104.4 (14)
C111—O11—P1	132.8 (8)	C247—C242—C243	110.0 (19)
C112—C111—C116	122.6 (10)	C247—C242—C241	133.0 (19)
C112—C111—O11	116.3 (11)	C243—C242—C241	116.9 (12)
C116—C111—O11	121.0 (8)	C244—C243—C242	118.2 (13)
C111—C112—C113	120.0 (11)	C244—C243—H243	120.9
C111—C112—C117	119.5 (12)	C242—C243—H243	120.9
C113—C112—C117	120.1 (12)	C243—C244—C245	127.8 (13)
C114—C113—C112	115.9 (11)	C243—C244—H244	116.1
C114—C113—H113	122.1	C245—C244—H244	116.1
C112—C113—H113	122.1	C244—C245—C246	115.3 (13)
C115—C114—C113	124.5 (12)	C244—C245—H245	122.3
C115—C114—H114	117.8	C246—C245—H245	122.3
C113—C114—H114	117.8	C241—C246—C245	117.8 (13)
C114—C115—C116	118.0 (11)	C241—C246—H246	121.1
C114—C115—H115	121	C245—C246—H246	121.1
C116—C115—H115	121	C242—C247—H24A	109.5
C111—C116—C115	118.5 (9)	C242—C247—H24B	109.5
C111—C116—H116	120.8	H24A—C247—H24B	109.5
C115—C116—H116	120.8	C242—C247—H24C	109.5
C112—C117—H11A	109.5	H24A—C247—H24C	109.5
C112—C117—H11B	109.5	H24B—C247—H24C	109.5
H11A—C117—H11B	109.5	C231—O23—P2	129.3 (8)
C112—C117—H11C	109.5	C236—C231—O23	122.9 (11)
H11A—C117—H11C	109.5	C236—C231—C232	123.5 (11)
H11B—C117—H11C	109.5	O23—C231—C232	113.4 (12)
C141—O41—P1	120.7 (7)	C233—C232—C231	113.8 (12)
C142—C141—O41	116.3 (9)	C233—C232—C237	128.7 (16)
C142—C141—C146	119.8 (8)	C231—C232—C237	117.5 (15)
O41—C141—C146	123.8 (8)	C234—C233—C232	123.3 (13)
C141—C142—C143	120.2 (10)	C234—C233—H233	118.3
C141—C142—C147	117.7 (9)	C232—C233—H233	118.3
C143—C142—C147	121.8 (10)	C233—C234—C235	121.8 (13)
C142—C143—C144	118.0 (9)	C233—C234—H234	119.1
C142—C143—H143	121	C235—C234—H234	119.1
C144—C143—H143	121	C236—C235—C234	115.1 (12)
C145—C144—C143	121.2 (10)	C236—C235—H235	122.4
C145—C144—H144	119.4	C234—C235—H235	122.4
C143—C144—H144	119.4	C231—C236—C235	121.9 (12)
C144—C145—C146	119.2 (10)	C231—C236—H236	119
C144—C145—H145	120.4	C235—C236—H236	119
C146—C145—H145	120.4	C232—C237—H23A	109.5
C141—C146—C145	120.7 (9)	C232—C237—H23B	109.5
C141—C146—H146	119.7	H23A—C237—H23B	109.5
C145—C146—H146	119.7	C232—C237—H23C	109.5
C142—C147—H14A	109.5	H23A—C237—H23C	109.5
C142—C147—H14B	109.5	H23B—C237—H23C	109.5
H14A—C147—H14B	109.5	C251—O25—P2'	128.3 (10)
C142—C147—H14C	109.5	O25—C251—C256	124.4 (10)
H14A—C147—H14C	109.5	O25—C251—C252	111.4 (10)
H14B—C147—H14C	109.5	C256—C251—C252	124.3 (8)
C121—O12—P1	125.9 (3)	C253—C252—C251	117.1 (8)
C126—C121—O12	122.4 (5)	C253—C252—C257	120.9 (9)
C126—C121—C122	122.6 (6)	C251—C252—C257	121.9 (9)
O12—C121—C122	115.0 (5)	C254—C253—C252	119.8 (9)
C121—C122—C123	116.4 (6)	C254—C253—H253	120.1
C121—C122—C127	121.5 (6)	C252—C253—H253	120.1
C123—C122—C127	122.0 (6)	C253—C254—C255	121.3 (10)
C124—C123—C122	121.9 (7)	C253—C254—H254	119.4
C124—C123—H123	119	C255—C254—H254	119.4
C122—C123—H123	119	C256—C255—C254	119.5 (10)
C123—C124—C125	120.1 (8)	C256—C255—H255	120.2
C123—C124—H124	119.9	C254—C255—H255	120.2
C125—C124—H124	119.9	C251—C256—C255	117.9 (9)
C124—C125—C126	119.7 (7)	C251—C256—H256	121.1
C124—C125—H125	120.1	C255—C256—H256	121.1
C126—C125—H125	120.1	C252—C257—H25A	109.5
C121—C126—C125	119.2 (6)	C252—C257—H25B	109.5
C121—C126—H126	120.4	H25A—C257—H25B	109.5
C125—C126—H126	120.4	C252—C257—H25C	109.5
C122—C127—H12A	109.5	H25A—C257—H25C	109.5
C122—C127—H12B	109.5	H25B—C257—H25C	109.5
H12A—C127—H12B	109.5	O33—P3—O31	96.93 (18)
C122—C127—H12C	109.5	O33—P3—O32	102.99 (18)
H12A—C127—H12C	109.5	O31—P3—O32	95.72 (19)
H12B—C127—H12C	109.5	O33—P3—Ni1	116.00 (13)
C131—O13—P1	124.7 (3)	O31—P3—Ni1	120.88 (15)
C132—C131—C136	122.2 (6)	O32—P3—Ni1	119.98 (14)
C132—C131—O13	118.2 (6)	C311—O31—P3	126.0 (3)
C136—C131—O13	119.6 (5)	C316—C311—C312	122.2 (5)
C131—C132—C133	117.0 (7)	C316—C311—O31	122.0 (5)
C131—C132—C137	120.8 (7)	C312—C311—O31	115.7 (5)
C133—C132—C137	122.2 (7)	C313—C312—C311	117.4 (5)
C134—C133—C132	121.3 (7)	C313—C312—C317	122.4 (5)
C134—C133—H133	119.3	C311—C312—C317	120.2 (5)
C132—C133—H133	119.3	C312—C313—C314	121.7 (6)
C135—C134—C133	120.4 (8)	C312—C313—H313	119.2
C135—C134—H134	119.8	C314—C313—H313	119.2
C133—C134—H134	119.8	C315—C314—C313	119.6 (6)
C134—C135—C136	120.1 (7)	C315—C314—H314	120.2
C134—C135—H135	120	C313—C314—H314	120.2
C136—C135—H135	120	C314—C315—C316	119.9 (5)
C135—C136—C131	119.0 (6)	C314—C315—H315	120
C135—C136—H136	120.5	C316—C315—H315	120
C131—C136—H136	120.5	C311—C316—C315	119.2 (5)
C132—C137—H13A	109.5	C311—C316—H316	120.4
C132—C137—H13B	109.5	C315—C316—H316	120.4
H13A—C137—H13B	109.5	C312—C317—H31A	109.5
C132—C137—H13C	109.5	C312—C317—H31B	109.5
H13A—C137—H13C	109.5	H31A—C317—H31B	109.5
H13B—C137—H13C	109.5	C312—C317—H31C	109.5
O22—P2—O21	98.9 (5)	H31A—C317—H31C	109.5
O22—P2—O23	92.4 (5)	H31B—C317—H31C	109.5
O21—P2—O23	99.0 (4)	C321—O32—P3	120.4 (3)
O22—P2—Ni1	121.7 (4)	C326—C321—C322	121.3 (5)
O21—P2—Ni1	120.5 (4)	C326—C321—O32	121.6 (5)
O23—P2—Ni1	118.6 (4)	C322—C321—O32	117.1 (5)
O25—P2'—O24	89.3 (8)	C321—C322—C323	116.4 (6)
O25—P2'—O21	101.5 (6)	C321—C322—C327	121.8 (5)
O24—P2'—O21	101.0 (6)	C323—C322—C327	121.8 (5)
O25—P2'—Ni1	131.4 (6)	C324—C323—C322	122.1 (6)
O24—P2'—Ni1	114.8 (6)	C324—C323—H323	118.9
O21—P2'—Ni1	113.2 (4)	C322—C323—H323	118.9
C211—O21—P2	127.5 (4)	C325—C324—C323	120.0 (6)
C211—O21—P2'	123.7 (4)	C325—C324—H324	120
C212—C211—C216	121.0 (5)	C323—C324—H324	120
C212—C211—O21	120.8 (4)	C324—C325—C326	119.8 (7)
C216—C211—O21	117.9 (5)	C324—C325—H325	120.1
C211—C212—C213	117.9 (6)	C326—C325—H325	120.1
C211—C212—C217	123.5 (5)	C321—C326—C325	120.4 (6)
C213—C212—C217	118.6 (6)	C321—C326—H326	119.8
C214—C213—C212	122.2 (7)	C325—C326—H326	119.8
C214—C213—H213	118.9	C322—C327—H32A	109.5
C212—C213—H213	118.9	C322—C327—H32B	109.5
C213—C214—C215	119.0 (6)	H32A—C327—H32B	109.5
C213—C214—H214	120.5	C322—C327—H32C	109.5
C215—C214—H214	120.5	H32A—C327—H32C	109.5
C216—C215—C214	120.6 (7)	H32B—C327—H32C	109.5
C216—C215—H215	119.7	C331—O33—P3	128.4 (3)
C214—C215—H215	119.7	C332—C331—C336	121.6 (5)
C215—C216—C211	119.4 (7)	C332—C331—O33	116.0 (4)
C215—C216—H216	120.3	C336—C331—O33	122.1 (4)
C211—C216—H216	120.3	C331—C332—C333	117.2 (6)
C212—C217—H21A	109.5	C331—C332—C337	121.4 (5)
C212—C217—H21B	109.5	C333—C332—C337	121.4 (6)
H21A—C217—H21B	109.5	C334—C333—C332	122.4 (6)
C212—C217—H21C	109.5	C334—C333—H333	118.8
H21A—C217—H21C	109.5	C332—C333—H333	118.8
H21B—C217—H21C	109.5	C335—C334—C333	118.8 (6)
C221—O22—P2	115.4 (6)	C335—C334—H334	120.6
O22—C221—C222	117.2 (9)	C333—C334—H334	120.6
O22—C221—C226	120.3 (8)	C334—C335—C336	120.1 (6)
C222—C221—C226	122.5 (9)	C334—C335—H335	120
C221—C222—C223	113.2 (9)	C336—C335—H335	120
C221—C222—C227	120.5 (11)	C331—C336—C335	119.9 (5)
C223—C222—C227	125.5 (11)	C331—C336—H336	120.1
C224—C223—C222	125.0 (12)	C335—C336—H336	120.1
C224—C223—H223	117.5	C332—C337—H33A	109.5
C222—C223—H223	117.5	C332—C337—H33B	109.5
C223—C224—C225	119.1 (12)	H33A—C337—H33B	109.5
C223—C224—H224	120.4	C332—C337—H33C	109.5
C225—C224—H224	120.4	H33A—C337—H33C	109.5
C226—C225—C224	119.1 (11)	H33B—C337—H33C	109.5
C226—C225—H225	120.5