Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100012075/qa0381sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270100012075/qa0381Isup2.hkl |
CCDC reference: 152649
The paramagnetic title compound, (I), was isolated from the products obtained in a metathesis reaction of LLi and (PPh3)2NiCl2 {L = [tBu2P(O)NEt]−} (Brück, 1995; Brück et al., 1996).
All H atoms have been calculated and included in a riding mode except for H3 which has been refined using a restrained N—H distance [N3—H3 0.853 (14) Å].
Data collection: Siemens/Bruker P3 (Siemens, 1989); cell refinement: Siemens/Bruker P3; data reduction: SHELXTL-Plus (Sheldrick, 1990); program(s) used to solve structure: SHELXTL-Plus; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXL97.
[NiLiCl(C10H23NOP)2(C10H24NOP)] | Dx = 1.123 Mg m−3 |
Mr = 714.90 | Melting point: 411 K K |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 17.304 (4) Å | Cell parameters from 40 reflections |
b = 13.055 (3) Å | θ = 10.0–12.6° |
c = 19.444 (4) Å | µ = 0.67 mm−1 |
β = 105.80 (2)° | T = 300 K |
V = 4226.5 (16) Å3 | Square bipyramid, metallic dark brown |
Z = 4 | 0.50 × 0.50 × 0.50 mm |
F(000) = 1548 |
Siemens/Bruker P3 diffractometer | Rint = 0.034 |
Radiation source: fine-focus sealed tube | θmax = 25.1°, θmin = 1.9° |
Graphite monochromator | h = 0→20 |
ω:2θ scans | k = 0→15 |
7746 measured reflections | l = −23→22 |
7461 independent reflections | 3 standard reflections every 100 reflections |
4206 reflections with I > 2σ(I) | intensity decay: 19% |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.133 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.93 | w = 1/[σ2(Fo2) + (0.0736P)2] where P = (Fo2 + 2Fc2)/3 |
7468 reflections | (Δ/σ)max < 0.001 |
421 parameters | Δρmax = 0.27 e Å−3 |
14 restraints | Δρmin = −0.25 e Å−3 |
[NiLiCl(C10H23NOP)2(C10H24NOP)] | V = 4226.5 (16) Å3 |
Mr = 714.90 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 17.304 (4) Å | µ = 0.67 mm−1 |
b = 13.055 (3) Å | T = 300 K |
c = 19.444 (4) Å | 0.50 × 0.50 × 0.50 mm |
β = 105.80 (2)° |
Siemens/Bruker P3 diffractometer | Rint = 0.034 |
7746 measured reflections | 3 standard reflections every 100 reflections |
7461 independent reflections | intensity decay: 19% |
4206 reflections with I > 2σ(I) |
R[F2 > 2σ(F2)] = 0.045 | 14 restraints |
wR(F2) = 0.133 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.93 | Δρmax = 0.27 e Å−3 |
7468 reflections | Δρmin = −0.25 e Å−3 |
421 parameters |
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. Several C atoms show enlarged displacement parameters of which the ethyl groups C3, C4, and C5, C6 could be described by split atom positions with refined s.o.f. of 0.64 (1), 0.36 (1) and 0.61 (1), 0.39 (1), resp. For reasonable distances and angles several DFIX had to be used for these groups. All H atoms have been calculated and included in a riding mode except atom H3 which has been refined free using a restrained distance. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ni | 0.49195 (3) | 0.25328 (3) | 0.24165 (2) | 0.05097 (16) | |
Cl | 0.47929 (7) | 0.33689 (9) | 0.33989 (6) | 0.0859 (4) | |
P1 | 0.53799 (6) | 0.02397 (7) | 0.27524 (5) | 0.0490 (2) | |
P2 | 0.41961 (6) | 0.29768 (7) | 0.10564 (5) | 0.0549 (3) | |
P3 | 0.23061 (6) | −0.07070 (8) | 0.06790 (6) | 0.0614 (3) | |
O1 | 0.46586 (15) | 0.00754 (17) | 0.21335 (13) | 0.0648 (7) | |
O2 | 0.40315 (14) | 0.20346 (17) | 0.14574 (11) | 0.0540 (6) | |
O3 | 0.29921 (15) | 0.00185 (19) | 0.08421 (14) | 0.0703 (8) | |
N1 | 0.56650 (16) | 0.1428 (2) | 0.27996 (13) | 0.0478 (7) | |
N2 | 0.4876 (2) | 0.3541 (2) | 0.16545 (16) | 0.0698 (10) | |
N3 | 0.1617 (3) | −0.0331 (3) | 0.1024 (3) | 0.1026 (14) | |
H3 | 0.125 (2) | −0.072 (3) | 0.109 (2) | 0.102 (18)* | |
C1 | 0.6410 (2) | 0.1782 (3) | 0.3313 (2) | 0.0709 (12) | |
H1A | 0.6732 | 0.1193 | 0.3519 | 0.085* | |
H1B | 0.6276 | 0.2153 | 0.3697 | 0.085* | |
C2 | 0.6892 (3) | 0.2466 (4) | 0.2963 (3) | 0.1094 (18) | |
H2A | 0.7372 | 0.2681 | 0.3312 | 0.131* | |
H2B | 0.6578 | 0.3055 | 0.2766 | 0.131* | |
H2C | 0.7034 | 0.2096 | 0.2588 | 0.131* | |
C3A | 0.5415 (9) | 0.4385 (8) | 0.1567 (7) | 0.118 (5) | 0.642 (15) |
H3A1 | 0.5202 | 0.4711 | 0.1106 | 0.142* | 0.642 (15) |
H3A2 | 0.5943 | 0.4115 | 0.1588 | 0.142* | 0.642 (15) |
C4A | 0.5477 (10) | 0.5163 (7) | 0.2161 (8) | 0.156 (7) | 0.642 (15) |
H4A1 | 0.5852 | 0.5689 | 0.2126 | 0.187* | 0.642 (15) |
H4A2 | 0.5658 | 0.4828 | 0.2616 | 0.187* | 0.642 (15) |
H4A3 | 0.4959 | 0.5464 | 0.2116 | 0.187* | 0.642 (15) |
C3B | 0.5012 (8) | 0.4663 (5) | 0.1723 (16) | 0.095 (7) | 0.358 (15) |
H3B1 | 0.4705 | 0.4952 | 0.2026 | 0.114* | 0.358 (15) |
H3B2 | 0.4834 | 0.4984 | 0.1257 | 0.114* | 0.358 (15) |
C4B | 0.5901 (9) | 0.4866 (12) | 0.205 (2) | 0.152 (14) | 0.358 (15) |
H4B1 | 0.6005 | 0.5586 | 0.2027 | 0.183* | 0.358 (15) |
H4B2 | 0.6206 | 0.4496 | 0.1784 | 0.183* | 0.358 (15) |
H4B3 | 0.6054 | 0.4643 | 0.2537 | 0.183* | 0.358 (15) |
C5A | 0.1334 (8) | 0.0735 (5) | 0.1078 (6) | 0.189 (8) | 0.613 (13) |
H5A1 | 0.0781 | 0.0805 | 0.0796 | 0.227* | 0.613 (13) |
H5A2 | 0.1660 | 0.1214 | 0.0898 | 0.227* | 0.613 (13) |
C6A | 0.1400 (16) | 0.0962 (12) | 0.1859 (7) | 0.274 (15) | 0.613 (13) |
H6A1 | 0.1229 | 0.1653 | 0.1904 | 0.329* | 0.613 (13) |
H6A2 | 0.1948 | 0.0883 | 0.2136 | 0.329* | 0.613 (13) |
H6A3 | 0.1066 | 0.0496 | 0.2030 | 0.329* | 0.613 (13) |
C5B | 0.1808 (7) | 0.0452 (10) | 0.1604 (7) | 0.111 (7) | 0.387 (13) |
H5B1 | 0.2295 | 0.0816 | 0.1599 | 0.133* | 0.387 (13) |
H5B2 | 0.1891 | 0.0123 | 0.2065 | 0.133* | 0.387 (13) |
C6B | 0.1108 (12) | 0.1196 (14) | 0.1479 (10) | 0.137 (9) | 0.387 (13) |
H6B1 | 0.1225 | 0.1714 | 0.1844 | 0.164* | 0.387 (13) |
H6B2 | 0.0631 | 0.0833 | 0.1496 | 0.164* | 0.387 (13) |
H6B3 | 0.1025 | 0.1512 | 0.1019 | 0.164* | 0.387 (13) |
C11 | 0.6179 (3) | −0.0630 (3) | 0.2603 (2) | 0.0694 (11) | |
C12 | 0.6890 (3) | −0.0848 (5) | 0.3255 (3) | 0.128 (2) | |
H12A | 0.7135 | −0.0213 | 0.3449 | 0.153* | |
H12B | 0.7277 | −0.1264 | 0.3113 | 0.153* | |
H12C | 0.6703 | −0.1203 | 0.3611 | 0.153* | |
C13 | 0.5818 (3) | −0.1661 (3) | 0.2326 (3) | 0.1100 (18) | |
H13A | 0.5616 | −0.1990 | 0.2683 | 0.132* | |
H13B | 0.6223 | −0.2084 | 0.2217 | 0.132* | |
H13C | 0.5386 | −0.1561 | 0.1901 | 0.132* | |
C14 | 0.6485 (4) | −0.0143 (4) | 0.2018 (3) | 0.116 (2) | |
H14A | 0.6716 | 0.0514 | 0.2176 | 0.139* | |
H14B | 0.6047 | −0.0057 | 0.1596 | 0.139* | |
H14C | 0.6885 | −0.0577 | 0.1911 | 0.139* | |
C15 | 0.5083 (2) | −0.0121 (3) | 0.3569 (2) | 0.0655 (11) | |
C16 | 0.5697 (3) | 0.0130 (5) | 0.4256 (2) | 0.136 (3) | |
H16A | 0.6180 | −0.0250 | 0.4285 | 0.163* | |
H16B | 0.5492 | −0.0049 | 0.4652 | 0.163* | |
H16C | 0.5813 | 0.0850 | 0.4272 | 0.163* | |
C17 | 0.4319 (3) | 0.0477 (4) | 0.3522 (3) | 0.1091 (18) | |
H17A | 0.3926 | 0.0314 | 0.3082 | 0.131* | |
H17B | 0.4433 | 0.1198 | 0.3536 | 0.131* | |
H17C | 0.4113 | 0.0299 | 0.3918 | 0.131* | |
C18 | 0.4852 (3) | −0.1253 (4) | 0.3570 (3) | 0.1098 (18) | |
H18A | 0.4456 | −0.1413 | 0.3132 | 0.132* | |
H18B | 0.4636 | −0.1385 | 0.3967 | 0.132* | |
H18C | 0.5320 | −0.1669 | 0.3612 | 0.132* | |
C21 | 0.4559 (3) | 0.2532 (4) | 0.0306 (2) | 0.0837 (13) | |
C22 | 0.5304 (4) | 0.1899 (6) | 0.0643 (3) | 0.169 (3) | |
H22A | 0.5167 | 0.1357 | 0.0923 | 0.202* | |
H22B | 0.5706 | 0.2329 | 0.0945 | 0.202* | |
H22C | 0.5509 | 0.1610 | 0.0274 | 0.202* | |
C23 | 0.3957 (5) | 0.1824 (6) | −0.0198 (3) | 0.178 (3) | |
H23A | 0.3800 | 0.1288 | 0.0074 | 0.214* | |
H23B | 0.4202 | 0.1529 | −0.0539 | 0.214* | |
H23C | 0.3492 | 0.2210 | −0.0444 | 0.214* | |
C24 | 0.4795 (5) | 0.3367 (5) | −0.0125 (3) | 0.160 (3) | |
H24A | 0.4334 | 0.3780 | −0.0342 | 0.192* | |
H24B | 0.5001 | 0.3070 | −0.0491 | 0.192* | |
H24C | 0.5202 | 0.3787 | 0.0181 | 0.192* | |
C25 | 0.3254 (3) | 0.3713 (3) | 0.0774 (2) | 0.0798 (13) | |
C26 | 0.3295 (4) | 0.4661 (4) | 0.0329 (4) | 0.148 (3) | |
H26A | 0.3415 | 0.4460 | −0.0106 | 0.178* | |
H26B | 0.3707 | 0.5111 | 0.0595 | 0.178* | |
H26C | 0.2787 | 0.5009 | 0.0216 | 0.178* | |
C27 | 0.2570 (3) | 0.3019 (5) | 0.0350 (4) | 0.154 (3) | |
H27A | 0.2682 | 0.2807 | −0.0086 | 0.184* | |
H27B | 0.2073 | 0.3392 | 0.0240 | 0.184* | |
H27C | 0.2529 | 0.2428 | 0.0631 | 0.184* | |
C28 | 0.3064 (4) | 0.4026 (6) | 0.1448 (3) | 0.170 (3) | |
H28A | 0.3039 | 0.3429 | 0.1730 | 0.204* | |
H28B | 0.2555 | 0.4372 | 0.1334 | 0.204* | |
H28C | 0.3475 | 0.4478 | 0.1714 | 0.204* | |
C31 | 0.2633 (3) | −0.1953 (3) | 0.1091 (3) | 0.0873 (14) | |
C32 | 0.2002 (3) | −0.2797 (4) | 0.0874 (4) | 0.130 (2) | |
H32A | 0.1517 | −0.2585 | 0.0983 | 0.156* | |
H32B | 0.2199 | −0.3412 | 0.1133 | 0.156* | |
H32C | 0.1892 | −0.2924 | 0.0371 | 0.156* | |
C33 | 0.2831 (5) | −0.1772 (5) | 0.1896 (3) | 0.169 (3) | |
H33A | 0.2355 | −0.1557 | 0.2019 | 0.203* | |
H33B | 0.3234 | −0.1250 | 0.2030 | 0.203* | |
H33C | 0.3028 | −0.2396 | 0.2143 | 0.203* | |
C34 | 0.3399 (3) | −0.2290 (4) | 0.0919 (4) | 0.147 (3) | |
H34A | 0.3796 | −0.1760 | 0.1055 | 0.176* | |
H34B | 0.3289 | −0.2417 | 0.0415 | 0.176* | |
H34C | 0.3596 | −0.2905 | 0.1177 | 0.176* | |
C35 | 0.1871 (4) | −0.0745 (5) | −0.0304 (3) | 0.1093 (19) | |
C36 | 0.1745 (4) | 0.0353 (5) | −0.0540 (3) | 0.177 (4) | |
H36A | 0.1372 | 0.0669 | −0.0320 | 0.212* | |
H36B | 0.1534 | 0.0379 | −0.1051 | 0.212* | |
H36C | 0.2248 | 0.0710 | −0.0401 | 0.212* | |
C37 | 0.1054 (4) | −0.1287 (6) | −0.0499 (4) | 0.197 (4) | |
H37A | 0.1124 | −0.1990 | −0.0351 | 0.236* | |
H37B | 0.0823 | −0.1256 | −0.1007 | 0.236* | |
H37C | 0.0703 | −0.0954 | −0.0263 | 0.236* | |
C38 | 0.2461 (5) | −0.1216 (7) | −0.0659 (3) | 0.196 (4) | |
H38A | 0.2553 | −0.1919 | −0.0515 | 0.235* | |
H38B | 0.2960 | −0.0847 | −0.0520 | 0.235* | |
H38C | 0.2247 | −0.1181 | −0.1169 | 0.235* | |
Li | 0.3848 (4) | 0.0645 (5) | 0.1458 (3) | 0.0569 (16) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni | 0.0534 (3) | 0.0439 (3) | 0.0478 (3) | −0.0026 (2) | 0.0004 (2) | 0.0020 (2) |
Cl | 0.0971 (9) | 0.0803 (8) | 0.0839 (8) | 0.0025 (7) | 0.0307 (7) | −0.0200 (6) |
P1 | 0.0493 (6) | 0.0463 (5) | 0.0459 (5) | 0.0046 (5) | 0.0036 (4) | 0.0061 (4) |
P2 | 0.0632 (7) | 0.0431 (5) | 0.0506 (5) | −0.0059 (5) | 0.0025 (5) | 0.0088 (4) |
P3 | 0.0530 (6) | 0.0479 (6) | 0.0773 (7) | −0.0143 (5) | 0.0078 (5) | −0.0047 (5) |
O1 | 0.0670 (17) | 0.0470 (14) | 0.0619 (16) | −0.0042 (13) | −0.0139 (13) | 0.0069 (12) |
O2 | 0.0567 (15) | 0.0430 (13) | 0.0532 (14) | −0.0073 (12) | −0.0006 (12) | 0.0094 (11) |
O3 | 0.0638 (17) | 0.0599 (16) | 0.0716 (17) | −0.0247 (13) | −0.0080 (14) | 0.0073 (13) |
N1 | 0.0439 (17) | 0.0503 (17) | 0.0434 (15) | −0.0035 (13) | 0.0020 (13) | 0.0007 (12) |
N2 | 0.077 (2) | 0.0510 (19) | 0.067 (2) | −0.0239 (17) | −0.0046 (17) | 0.0134 (15) |
N3 | 0.106 (3) | 0.052 (2) | 0.168 (4) | −0.019 (2) | 0.068 (3) | −0.020 (3) |
C1 | 0.055 (2) | 0.070 (3) | 0.074 (3) | −0.005 (2) | −0.005 (2) | 0.003 (2) |
C2 | 0.072 (3) | 0.121 (4) | 0.124 (4) | −0.043 (3) | 0.007 (3) | 0.012 (3) |
C3A | 0.128 (12) | 0.088 (7) | 0.114 (10) | −0.050 (8) | −0.008 (8) | 0.027 (7) |
C4A | 0.239 (18) | 0.077 (8) | 0.120 (9) | −0.068 (11) | −0.004 (13) | 0.006 (8) |
C3B | 0.136 (19) | 0.037 (8) | 0.096 (13) | −0.037 (10) | 0.004 (14) | −0.001 (8) |
C4B | 0.106 (15) | 0.054 (11) | 0.25 (3) | −0.023 (11) | −0.038 (18) | −0.011 (14) |
C5A | 0.109 (11) | 0.090 (10) | 0.38 (3) | 0.011 (8) | 0.091 (14) | 0.012 (12) |
C6A | 0.47 (4) | 0.143 (16) | 0.144 (16) | −0.02 (2) | −0.020 (19) | −0.064 (12) |
C5B | 0.091 (12) | 0.104 (14) | 0.149 (17) | 0.008 (10) | 0.050 (11) | −0.038 (12) |
C6B | 0.132 (15) | 0.119 (15) | 0.149 (18) | 0.070 (11) | 0.020 (14) | −0.080 (14) |
C11 | 0.079 (3) | 0.066 (3) | 0.063 (2) | 0.016 (2) | 0.020 (2) | 0.000 (2) |
C12 | 0.093 (4) | 0.151 (6) | 0.124 (4) | 0.064 (4) | 0.004 (3) | −0.010 (4) |
C13 | 0.126 (5) | 0.063 (3) | 0.142 (5) | 0.027 (3) | 0.039 (4) | −0.009 (3) |
C14 | 0.155 (5) | 0.093 (4) | 0.131 (5) | 0.034 (4) | 0.092 (4) | 0.007 (3) |
C15 | 0.063 (3) | 0.068 (3) | 0.066 (3) | 0.007 (2) | 0.020 (2) | 0.018 (2) |
C16 | 0.128 (5) | 0.230 (8) | 0.050 (3) | −0.047 (5) | 0.026 (3) | 0.003 (4) |
C17 | 0.114 (4) | 0.088 (4) | 0.154 (5) | 0.020 (3) | 0.085 (4) | 0.034 (3) |
C18 | 0.139 (5) | 0.079 (3) | 0.121 (4) | −0.002 (3) | 0.051 (4) | 0.041 (3) |
C21 | 0.103 (4) | 0.088 (3) | 0.064 (3) | −0.004 (3) | 0.029 (3) | 0.011 (3) |
C22 | 0.176 (7) | 0.230 (8) | 0.127 (5) | 0.104 (7) | 0.086 (5) | 0.045 (5) |
C23 | 0.262 (10) | 0.183 (7) | 0.107 (5) | −0.062 (7) | 0.079 (6) | −0.065 (5) |
C24 | 0.218 (8) | 0.159 (6) | 0.142 (5) | 0.002 (6) | 0.115 (6) | 0.053 (5) |
C25 | 0.082 (3) | 0.066 (3) | 0.076 (3) | 0.016 (2) | −0.003 (3) | 0.019 (2) |
C26 | 0.179 (6) | 0.089 (4) | 0.163 (6) | 0.050 (4) | 0.025 (5) | 0.052 (4) |
C27 | 0.094 (4) | 0.136 (5) | 0.186 (7) | 0.006 (4) | −0.040 (4) | 0.017 (5) |
C28 | 0.144 (6) | 0.232 (9) | 0.134 (6) | 0.121 (6) | 0.039 (5) | 0.016 (6) |
C31 | 0.080 (3) | 0.061 (3) | 0.125 (4) | −0.008 (3) | 0.035 (3) | 0.008 (3) |
C32 | 0.121 (5) | 0.055 (3) | 0.234 (7) | −0.017 (3) | 0.081 (5) | 0.001 (4) |
C33 | 0.246 (9) | 0.115 (5) | 0.124 (5) | 0.010 (5) | 0.011 (6) | 0.059 (4) |
C34 | 0.093 (4) | 0.098 (4) | 0.254 (8) | 0.020 (4) | 0.055 (5) | 0.042 (5) |
C35 | 0.103 (4) | 0.112 (4) | 0.087 (4) | −0.043 (4) | −0.018 (3) | −0.009 (3) |
C36 | 0.188 (7) | 0.143 (6) | 0.132 (5) | −0.033 (6) | −0.072 (5) | 0.049 (5) |
C37 | 0.143 (6) | 0.215 (8) | 0.179 (7) | −0.107 (6) | −0.048 (5) | −0.022 (6) |
C38 | 0.251 (10) | 0.251 (10) | 0.098 (5) | −0.024 (8) | 0.068 (6) | −0.039 (6) |
Li | 0.056 (4) | 0.052 (3) | 0.054 (3) | −0.012 (3) | 0.001 (3) | 0.008 (3) |
Ni—N1 | 1.943 (3) | N3—C5B | 1.490 (5) |
Ni—N2 | 1.967 (3) | C1—C2 | 1.505 (6) |
Ni—O2 | 2.168 (2) | C3A—C4A | 1.520 (5) |
Ni—Cl | 2.2620 (12) | C3B—C4B | 1.520 (5) |
P1—O1 | 1.495 (2) | C5A—C6A | 1.520 (5) |
P1—N1 | 1.623 (3) | C5B—C6B | 1.520 (5) |
P1—C15 | 1.858 (4) | C11—C14 | 1.520 (6) |
P1—C11 | 1.871 (4) | C11—C13 | 1.521 (6) |
P2—O2 | 1.524 (2) | C11—C12 | 1.533 (6) |
P2—N2 | 1.592 (3) | C15—C16 | 1.500 (6) |
P2—C21 | 1.832 (5) | C15—C17 | 1.517 (6) |
P2—C25 | 1.842 (4) | C15—C18 | 1.530 (6) |
P3—O3 | 1.484 (2) | C21—C24 | 1.499 (6) |
P3—N3 | 1.596 (4) | C21—C22 | 1.522 (7) |
P3—C31 | 1.833 (5) | C21—C23 | 1.531 (7) |
P3—C35 | 1.854 (5) | C25—C28 | 1.493 (7) |
O1—Li | 1.801 (6) | C25—C26 | 1.524 (6) |
O2—Li | 1.842 (6) | C25—C27 | 1.539 (7) |
O3—Li | 1.824 (6) | C31—C34 | 1.518 (7) |
N1—C1 | 1.473 (4) | C31—C33 | 1.527 (7) |
N2—C3A | 1.483 (5) | C31—C32 | 1.527 (6) |
N2—C3B | 1.484 (5) | C35—C36 | 1.502 (8) |
N3—H3 | 0.853 (14) | C35—C38 | 1.512 (9) |
N3—C5A | 1.488 (5) | C35—C37 | 1.533 (7) |
N1—Ni—N2 | 132.09 (14) | N1—C1—C2 | 111.7 (3) |
N1—Ni—O2 | 110.37 (10) | N2—C3A—C4A | 109.0 (5) |
N2—Ni—O2 | 71.34 (10) | N2—C3B—C4B | 109.1 (5) |
N1—Ni—Cl | 103.96 (9) | N3—C5A—C6A | 108.5 (5) |
N2—Ni—Cl | 108.71 (11) | N3—C5B—C6B | 108.4 (5) |
O2—Ni—Cl | 131.46 (8) | C14—C11—C13 | 107.3 (4) |
O1—P1—N1 | 110.92 (13) | C14—C11—C12 | 109.4 (4) |
O1—P1—C15 | 106.67 (18) | C13—C11—C12 | 106.8 (4) |
N1—P1—C15 | 110.15 (17) | C14—C11—P1 | 106.6 (3) |
O1—P1—C11 | 106.18 (17) | C13—C11—P1 | 110.0 (3) |
N1—P1—C11 | 111.26 (18) | C12—C11—P1 | 116.4 (3) |
C15—P1—C11 | 111.51 (18) | C16—C15—C17 | 109.6 (4) |
O2—P2—N2 | 101.73 (14) | C16—C15—C18 | 109.4 (4) |
O2—P2—C21 | 107.68 (18) | C17—C15—C18 | 105.9 (4) |
N2—P2—C21 | 112.5 (2) | C16—C15—P1 | 114.3 (3) |
O2—P2—C25 | 107.43 (18) | C17—C15—P1 | 104.9 (3) |
N2—P2—C25 | 113.2 (2) | C18—C15—P1 | 112.2 (3) |
C21—P2—C25 | 113.3 (2) | C24—C21—C22 | 108.0 (5) |
O3—P3—N3 | 111.1 (2) | C24—C21—C23 | 108.9 (5) |
O3—P3—C31 | 109.85 (19) | C22—C21—C23 | 107.2 (5) |
N3—P3—C31 | 105.4 (2) | C24—C21—P2 | 114.8 (4) |
O3—P3—C35 | 108.3 (2) | C22—C21—P2 | 105.3 (3) |
N3—P3—C35 | 107.5 (3) | C23—C21—P2 | 112.3 (4) |
C31—P3—C35 | 114.6 (3) | C28—C25—C26 | 109.4 (5) |
P1—O1—Li | 147.3 (2) | C28—C25—C27 | 108.1 (5) |
P2—O2—Li | 148.4 (2) | C26—C25—C27 | 108.7 (4) |
P2—O2—Ni | 90.60 (11) | C28—C25—P2 | 105.7 (3) |
Li—O2—Ni | 112.2 (2) | C26—C25—P2 | 114.7 (4) |
P3—O3—Li | 152.3 (3) | C27—C25—P2 | 110.0 (3) |
C1—N1—P1 | 122.3 (2) | C34—C31—C33 | 107.8 (5) |
C1—N1—Ni | 113.2 (2) | C34—C31—C32 | 109.4 (4) |
P1—N1—Ni | 121.88 (15) | C33—C31—C32 | 109.8 (5) |
C3A—N2—C3B | 35.7 (7) | C34—C31—P3 | 110.1 (4) |
C3A—N2—P2 | 128.5 (6) | C33—C31—P3 | 105.5 (4) |
C3B—N2—P2 | 126.1 (8) | C32—C31—P3 | 114.1 (4) |
C3A—N2—Ni | 133.4 (7) | C36—C35—C38 | 107.9 (6) |
C3B—N2—Ni | 128.3 (12) | C36—C35—C37 | 108.5 (6) |
P2—N2—Ni | 96.32 (13) | C38—C35—C37 | 113.0 (6) |
H3—N3—C5A | 106 (3) | C36—C35—P3 | 105.9 (4) |
H3—N3—C5B | 108 (3) | C38—C35—P3 | 110.3 (4) |
C5A—N3—C5B | 46.7 (7) | C37—C35—P3 | 110.9 (5) |
H3—N3—P3 | 124 (3) | O1—Li—O3 | 128.7 (4) |
C5A—N3—P3 | 128.0 (6) | O1—Li—O2 | 107.9 (3) |
C5B—N3—P3 | 119.5 (6) | O3—Li—O2 | 123.4 (3) |
Experimental details
Crystal data | |
Chemical formula | [NiLiCl(C10H23NOP)2(C10H24NOP)] |
Mr | 714.90 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 300 |
a, b, c (Å) | 17.304 (4), 13.055 (3), 19.444 (4) |
β (°) | 105.80 (2) |
V (Å3) | 4226.5 (16) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.67 |
Crystal size (mm) | 0.50 × 0.50 × 0.50 |
Data collection | |
Diffractometer | Siemens/Bruker P3 diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7746, 7461, 4206 |
Rint | 0.034 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.045, 0.133, 0.93 |
No. of reflections | 7468 |
No. of parameters | 421 |
No. of restraints | 14 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.27, −0.25 |
Computer programs: Siemens/Bruker P3 (Siemens, 1989), Siemens/Bruker P3, SHELXTL-Plus (Sheldrick, 1990), SHELXTL-Plus, SHELXL97 (Sheldrick, 1997), SHELXL97.
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The paramagnetic (µeff=3.3 BM at 300 K) title compound, (I), revealed an incomplete bischelation of Ni2+ by L− with formation of a pseudo-tetrahedral NiON2Cl chromophore. The Ni atom is coordinated by Cl−, bidentate L− and monodentate LLi (via N). The coordination is pseudo-tetrahedral with a dihedral angle of 68.8 (1)° between the planes defined by Ni/O2/N2 and Ni/Cl/N1. A trigonal–planar LiO3 coordination [angles at Li of 107.9 (3), 123.4 (3) and 128.7 (3)°] is formed by bonds between Li and the pendant ligand [1.801 (6) Å], L− [1.842 (6) Å] and the protonated L− [1.825 (6) Å]. Preliminary results have been reported elsewhere (Wunderlich, 1996).