Download citation
Download citation
link to html
The crystal structure of the title compound, [tBu2P(S)NiPr]2Ni or [Ni(C11H25NPS)2], shows a dihedral angle of 82.27 (6)° between the two Ni/S/N planes and thus a distorted tetrahedral arrangement of the NiN2S2 chromophore. The structure is in accordance with the observed paramagnetism and is contrasted with the oxo analogue, which is planar but also paramagnetic.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100011264/jz1401sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100011264/jz1401Isup2.hkl
Contains datablock I

CCDC reference: 153866

Computing details top

Data collection: P3 (Siemens, 1993); cell refinement: P3; data reduction: SHELXTL-Plus (Sheldrick, 1990); program(s) used to solve structure: SHELXTL-Plus; program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus; software used to prepare material for publication: SHELXL97.

Bis(P,P-di-tert-butylthiophosphinic-N-isopropylamidato-N,S)nickel(II) top
Crystal data top
C22H50N2NiP2S2Dx = 1.176 Mg m3
Mr = 527.41Melting point: 407 K
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 16.123 (2) ÅCell parameters from 32 reflections
b = 11.684 (1) Åθ = 14.1–17.0°
c = 15.815 (2) ŵ = 0.91 mm1
β = 90.74 (1)°T = 300 K
V = 2979.0 (6) Å3Polyhedron, metallic intense blue
Z = 40.50 × 0.45 × 0.45 mm
F(000) = 1144
Data collection top
Siemens/Bruker P3
diffractometer
Rint = 0.000
Radiation source: fine-focus sealed tubeθmax = 27.6°, θmin = 2.2°
Graphite monochromatorh = 2020
ω–2θ scansk = 150
6844 measured reflectionsl = 020
6844 independent reflections3 standard reflections every 100 reflections
4889 reflections with I > 2σ(I) intensity decay: 14%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.039Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.116H atoms treated by a mixture of independent and constrained refinement
S = 1.00 w = [σ2(Fo2) + (0.0723P)2]
where P = Fo2 + 2Fc2)/3
6844 reflections(Δ/σ)max < 0.001
263 parametersΔρmax = 0.45 e Å3
0 restraintsΔρmin = 0.49 e Å3
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
xyzUiso*/Ueq
Ni0.251038 (18)0.11069 (2)0.178323 (18)0.03863 (11)
S10.38047 (4)0.17682 (6)0.23412 (5)0.0580 (2)
S20.12902 (5)0.10909 (6)0.26158 (5)0.0627 (2)
P10.35848 (4)0.28310 (5)0.13636 (4)0.04049 (16)
P20.14585 (4)0.05723 (5)0.23521 (4)0.04095 (16)
N10.27274 (12)0.23254 (16)0.09830 (12)0.0401 (4)
N20.22661 (12)0.05205 (16)0.17676 (12)0.0413 (4)
C10.22290 (16)0.2724 (2)0.02567 (16)0.0542 (6)
H10.25100.33790.00000.081*
C20.27440 (18)0.1451 (2)0.1372 (2)0.0604 (7)
H20.24730.21830.14940.091*
C30.13709 (19)0.3095 (4)0.0522 (2)0.0856 (11)
H3A0.10620.33500.00340.128*
H3B0.14170.37100.09220.128*
H3C0.10900.24610.07770.128*
C40.2148 (2)0.1778 (4)0.0403 (2)0.0887 (11)
H4A0.18210.20480.08740.133*
H4B0.18820.11250.01560.133*
H4C0.26890.15640.05940.133*
C50.2754 (3)0.1274 (4)0.0417 (2)0.1010 (14)
H5A0.30670.18770.01600.152*
H5B0.30070.05500.02930.152*
H5C0.21960.12830.01990.152*
C60.3624 (2)0.1488 (3)0.1718 (3)0.0819 (10)
H6A0.39210.20970.14510.123*
H6B0.36140.16160.23170.123*
H6C0.38940.07730.16050.123*
C110.44588 (16)0.2715 (3)0.0598 (2)0.0614 (7)
C120.5287 (2)0.3056 (4)0.1008 (3)0.1073 (15)
H12A0.52700.38500.11630.161*
H12B0.57260.29340.06140.161*
H12C0.53840.25990.15030.161*
C130.4514 (2)0.1444 (3)0.0357 (3)0.1011 (14)
H13A0.40000.12060.00980.152*
H13B0.46180.09960.08560.152*
H13C0.49570.13350.00340.152*
C140.4311 (2)0.3420 (4)0.0206 (2)0.0939 (12)
H14A0.37900.32050.04600.141*
H14B0.47500.32780.05970.141*
H14C0.42990.42190.00650.141*
C150.3461 (2)0.4310 (2)0.1799 (2)0.0612 (7)
C160.2714 (3)0.4251 (3)0.2385 (3)0.0944 (13)
H16A0.22330.40080.20690.142*
H16B0.26150.49940.26230.142*
H16C0.28260.37140.28320.142*
C170.4218 (3)0.4692 (4)0.2316 (3)0.1245 (18)
H17A0.46920.47330.19560.187*
H17B0.43230.41510.27620.187*
H17C0.41140.54320.25560.187*
C180.3276 (3)0.5193 (3)0.1110 (3)0.0989 (13)
H18A0.37380.52400.07350.148*
H18B0.31840.59270.13650.148*
H18C0.27890.49680.07960.148*
C210.05239 (18)0.1130 (3)0.17779 (19)0.0646 (8)
C220.0266 (2)0.1002 (4)0.2286 (3)0.0925 (12)
H22A0.02220.14530.27920.139*
H22B0.07320.12590.19530.139*
H22C0.03420.02120.24330.139*
C230.0614 (2)0.2377 (4)0.1512 (2)0.0944 (13)
H23A0.06700.28490.20070.142*
H23B0.10980.24600.11700.142*
H23C0.01320.26080.11940.142*
C240.0438 (2)0.0401 (5)0.0981 (3)0.130 (2)
H24A0.09320.04710.06510.194*
H24B0.03600.03850.11360.194*
H24C0.00310.06590.06530.194*
C250.1664 (2)0.1351 (3)0.33711 (18)0.0668 (8)
C260.2419 (3)0.0788 (4)0.3762 (2)0.0969 (13)
H26A0.28780.08590.33860.145*
H26B0.25530.11540.42900.145*
H26C0.23050.00070.38590.145*
C270.0953 (3)0.1205 (5)0.3987 (3)0.134 (2)
H27A0.04600.15520.37550.201*
H27B0.08560.04050.40810.201*
H27C0.10950.15670.45140.201*
C280.1864 (4)0.2616 (3)0.3223 (3)0.139 (2)
H28A0.13920.29880.29690.209*
H28B0.19960.29750.37540.209*
H28C0.23300.26770.28540.209*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.04046 (17)0.03194 (16)0.0436 (2)0.00542 (12)0.00397 (12)0.00163 (12)
S10.0592 (4)0.0533 (4)0.0608 (4)0.0119 (3)0.0195 (3)0.0138 (3)
S20.0620 (4)0.0412 (3)0.0856 (6)0.0044 (3)0.0314 (4)0.0015 (3)
P10.0397 (3)0.0360 (3)0.0458 (4)0.0071 (2)0.0018 (2)0.0013 (3)
P20.0439 (3)0.0367 (3)0.0422 (4)0.0074 (3)0.0010 (2)0.0055 (2)
N10.0403 (10)0.0412 (10)0.0388 (10)0.0058 (8)0.0011 (8)0.0058 (8)
N20.0421 (10)0.0312 (10)0.0506 (11)0.0045 (8)0.0021 (8)0.0046 (8)
C10.0513 (14)0.0633 (17)0.0480 (14)0.0076 (13)0.0049 (11)0.0168 (13)
C20.0642 (17)0.0350 (13)0.082 (2)0.0019 (12)0.0106 (15)0.0182 (13)
C30.0535 (18)0.105 (3)0.098 (3)0.0106 (18)0.0118 (17)0.027 (2)
C40.096 (3)0.115 (3)0.0553 (18)0.001 (2)0.0227 (18)0.010 (2)
C50.115 (3)0.112 (3)0.076 (2)0.006 (3)0.023 (2)0.048 (2)
C60.0601 (19)0.067 (2)0.119 (3)0.0173 (16)0.0071 (19)0.019 (2)
C110.0432 (14)0.0669 (19)0.0746 (18)0.0122 (13)0.0166 (13)0.0029 (15)
C120.0465 (18)0.151 (4)0.124 (3)0.024 (2)0.012 (2)0.010 (3)
C130.081 (2)0.082 (3)0.142 (4)0.003 (2)0.057 (3)0.030 (2)
C140.089 (3)0.123 (3)0.070 (2)0.013 (2)0.0343 (19)0.014 (2)
C150.0753 (19)0.0394 (14)0.0690 (18)0.0108 (13)0.0072 (15)0.0062 (13)
C160.130 (3)0.061 (2)0.094 (3)0.004 (2)0.044 (2)0.0289 (19)
C170.116 (3)0.081 (3)0.175 (5)0.020 (3)0.038 (3)0.057 (3)
C180.145 (4)0.0401 (18)0.112 (3)0.009 (2)0.027 (3)0.0143 (18)
C210.0521 (15)0.081 (2)0.0604 (17)0.0282 (15)0.0067 (13)0.0144 (15)
C220.0496 (18)0.105 (3)0.123 (3)0.0177 (18)0.0040 (19)0.006 (2)
C230.084 (2)0.108 (3)0.091 (3)0.045 (2)0.001 (2)0.034 (2)
C240.088 (3)0.200 (5)0.099 (3)0.063 (3)0.052 (2)0.077 (3)
C250.092 (2)0.0617 (18)0.0470 (15)0.0068 (16)0.0073 (15)0.0125 (13)
C260.113 (3)0.116 (3)0.061 (2)0.002 (3)0.032 (2)0.002 (2)
C270.125 (4)0.206 (6)0.072 (3)0.015 (4)0.027 (3)0.055 (3)
C280.273 (7)0.054 (2)0.088 (3)0.008 (3)0.043 (4)0.027 (2)
Geometric parameters (Å, º) top
Ni—N11.9397 (18)C1—C41.524 (4)
Ni—N21.9419 (19)C2—C61.514 (4)
Ni—S22.3814 (8)C2—C51.525 (5)
Ni—S12.3839 (8)C11—C141.531 (5)
S1—P12.0109 (9)C11—C121.529 (4)
S2—P22.0067 (10)C11—C131.536 (5)
P1—N11.6126 (19)C15—C171.527 (5)
P1—C151.871 (3)C15—C181.528 (5)
P1—C111.875 (3)C15—C161.531 (5)
P2—N21.608 (2)C21—C221.522 (5)
P2—C211.867 (3)C21—C241.527 (5)
P2—C251.877 (3)C21—C231.523 (5)
N1—C11.469 (3)C25—C261.509 (5)
N2—C21.476 (3)C25—C271.524 (5)
C1—C31.514 (4)C25—C281.531 (5)
N1—Ni—N2138.48 (8)C3—C1—C4109.1 (3)
N1—Ni—S2121.59 (6)N2—C2—C6111.1 (2)
N2—Ni—S280.24 (6)N2—C2—C5109.4 (3)
N1—Ni—S180.74 (6)C6—C2—C5109.8 (3)
N2—Ni—S1119.90 (6)C14—C11—C12109.7 (3)
S2—Ni—S1121.56 (3)C14—C11—C13108.8 (3)
P1—S1—Ni76.75 (3)C12—C11—C13107.7 (3)
P2—S2—Ni77.16 (3)C14—C11—P1112.8 (2)
N1—P1—C15112.35 (12)C12—C11—P1111.5 (2)
N1—P1—C11112.35 (12)C13—C11—P1106.0 (2)
C15—P1—C11112.90 (13)C17—C15—C18109.4 (3)
N1—P1—S1101.68 (7)C17—C15—C16108.5 (3)
C15—P1—S1107.83 (10)C18—C15—C16108.3 (3)
C11—P1—S1108.98 (11)C17—C15—P1112.3 (2)
N2—P2—C21112.84 (12)C18—C15—P1112.5 (2)
N2—P2—C25112.13 (13)C16—C15—P1105.7 (2)
C21—P2—C25112.38 (14)C22—C21—C24108.3 (3)
N2—P2—S2101.29 (7)C22—C21—C23108.9 (3)
C21—P2—S2109.21 (11)C24—C21—C23108.3 (3)
C25—P2—S2108.31 (11)C22—C21—P2112.6 (2)
C1—N1—P1129.31 (17)C24—C21—P2105.7 (2)
C1—N1—Ni129.88 (16)C23—C21—P2112.9 (2)
P1—N1—Ni100.74 (9)C26—C25—C27107.4 (3)
C2—N2—P2130.30 (17)C26—C25—C28108.2 (4)
C2—N2—Ni128.29 (17)C27—C25—C28111.6 (4)
P2—N2—Ni101.25 (10)C26—C25—P2105.8 (2)
N1—C1—C3111.5 (2)C27—C25—P2111.6 (3)
N1—C1—C4110.3 (2)C28—C25—P2111.8 (2)
 

Follow Acta Cryst. C
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds