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The title complex, [Ni(C6H4ClS)2(C12H27P3)2], resides on a crystallographic inversion center in a triclinic unit cell. The structural features of the complex compare well with those of similar square planar Ni(O) complexes reported in the Cambridge Structural Database.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801018554/wn6066sup1.cif
Contains datablocks dar02, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801018554/wn6066Isup2.hkl
Contains datablock I

CCDC reference: 177178

Key indicators

  • Single-crystal X-ray study
  • T = 173 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.043
  • wR factor = 0.126
  • Data-to-parameter ratio = 19.3

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Yellow Alert Alert Level C:
REFLT_03 From the CIF: _diffrn_reflns_theta_max 26.37 From the CIF: _reflns_number_total 3843 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 4171 Completeness (_total/calc) 92.14% Alert C: < 95% complete
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SHELXTL (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

(I) top
Crystal data top
C36H62Cl2NiP2S2Z = 1
Mr = 750.53F(000) = 402
Triclinic, P1Dx = 1.220 Mg m3
a = 8.6314 (7) ÅMo Kα radiation, λ = 0.71073 Å
b = 10.3062 (8) ÅCell parameters from 564 reflections
c = 11.9720 (9) Åθ = 2.0–24.0°
α = 75.4198 (10)°µ = 0.81 mm1
β = 83.3078 (10)°T = 173 K
γ = 84.9883 (10)°Block, red
V = 1021.81 (14) Å30.50 × 0.40 × 0.40 mm
Data collection top
CCD area-detector
diffractometer
3843 independent reflections
Radiation source: fine-focus sealed tube3133 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.000
phi and ω scansθmax = 26.4°, θmin = 1.8°
Absorption correction: empirical
(SADABS; Blessing, 1995)
h = 1010
Tmin = 0.688, Tmax = 0.738k = 1212
3843 measured reflectionsl = 014
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)] = 0.043Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.126H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0676P)2 + 0.4884P]
where P = (Fo2 + 2Fc2)/3
3843 reflections(Δ/σ)max < 0.001
199 parametersΔρmax = 1.80 e Å3
0 restraintsΔρmin = 0.45 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
Ni0.50001.00001.00000.02636 (16)
Cl0.05114 (13)1.23270 (14)1.43178 (10)0.0810 (4)
S10.31798 (8)1.16564 (7)0.96548 (7)0.0354 (2)
P10.35809 (8)0.88901 (7)0.91402 (6)0.02870 (19)
C10.2195 (3)1.1784 (3)1.0989 (3)0.0358 (7)
C20.2107 (3)1.0730 (3)1.1969 (3)0.0416 (7)
H20.26140.98841.19330.050*
C30.1298 (4)1.0881 (4)1.3003 (3)0.0523 (9)
H30.12521.01531.36720.063*
C40.0554 (4)1.2127 (4)1.3034 (3)0.0533 (9)
C50.0616 (4)1.3188 (4)1.2082 (4)0.0541 (9)
H50.00991.40281.21280.065*
C60.1428 (3)1.3041 (3)1.1059 (3)0.0449 (8)
H60.14751.37811.03980.054*
C70.2730 (3)0.9878 (3)0.7838 (3)0.0364 (7)
H7A0.22000.92720.75020.044*
H7B0.19281.05390.80600.044*
C80.3922 (4)1.0619 (3)0.6918 (3)0.0416 (7)
H8A0.47430.99640.67100.050*
H8B0.44271.12510.72420.050*
C90.3190 (5)1.1398 (4)0.5828 (3)0.0607 (10)
H9A0.26981.07600.55030.073*
H9B0.23541.20360.60440.073*
C100.4329 (6)1.2163 (5)0.4906 (3)0.0860 (15)
H10A0.48021.28170.52120.129*
H10B0.37811.26350.42340.129*
H10C0.51491.15380.46720.129*
C110.4451 (3)0.7374 (3)0.8717 (2)0.0313 (6)
H11A0.53730.76330.81530.038*
H11B0.48400.67480.94140.038*
C120.3426 (3)0.6604 (3)0.8188 (3)0.0363 (7)
H12A0.30720.71950.74630.044*
H12B0.24890.63420.87340.044*
C130.4302 (4)0.5348 (3)0.7923 (3)0.0394 (7)
H13A0.53380.55920.75110.047*
H13B0.44780.46900.86640.047*
C140.3451 (5)0.4689 (3)0.7192 (3)0.0548 (9)
H14A0.24640.43720.76230.082*
H14B0.41040.39270.70130.082*
H14C0.32370.53440.64690.082*
C150.1870 (3)0.8321 (3)1.0142 (3)0.0351 (6)
H15A0.12830.91081.03520.042*
H15B0.11760.79080.97440.042*
C160.2288 (3)0.7305 (3)1.1251 (3)0.0376 (7)
H16A0.26580.64411.10630.045*
H16B0.31580.76321.15560.045*
C170.0916 (4)0.7065 (3)1.2191 (3)0.0482 (8)
H17A0.05230.79331.23630.058*
H17B0.00590.67071.18970.058*
C180.1359 (5)0.6088 (4)1.3304 (3)0.0632 (10)
H18A0.17820.52361.31340.095*
H18B0.04310.59281.38630.095*
H18C0.21510.64681.36310.095*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.0223 (3)0.0269 (3)0.0312 (3)0.00032 (19)0.00663 (19)0.0084 (2)
Cl0.0665 (7)0.1186 (10)0.0648 (7)0.0182 (6)0.0032 (5)0.0446 (7)
S10.0316 (4)0.0327 (4)0.0442 (4)0.0055 (3)0.0133 (3)0.0121 (3)
P10.0251 (4)0.0288 (4)0.0339 (4)0.0004 (3)0.0088 (3)0.0086 (3)
C10.0220 (13)0.0385 (16)0.0534 (19)0.0017 (12)0.0098 (13)0.0206 (14)
C20.0306 (15)0.0439 (17)0.055 (2)0.0039 (13)0.0055 (14)0.0202 (16)
C30.0405 (18)0.065 (2)0.058 (2)0.0077 (17)0.0049 (16)0.0248 (18)
C40.0337 (17)0.078 (3)0.060 (2)0.0004 (17)0.0045 (16)0.041 (2)
C50.0360 (18)0.060 (2)0.081 (3)0.0078 (16)0.0152 (18)0.043 (2)
C60.0305 (15)0.0481 (18)0.065 (2)0.0030 (14)0.0139 (15)0.0283 (17)
C70.0390 (16)0.0337 (15)0.0404 (16)0.0028 (13)0.0176 (13)0.0115 (13)
C80.0507 (19)0.0390 (16)0.0369 (17)0.0020 (14)0.0122 (14)0.0102 (13)
C90.086 (3)0.055 (2)0.040 (2)0.003 (2)0.0218 (19)0.0049 (17)
C100.140 (5)0.068 (3)0.042 (2)0.005 (3)0.005 (3)0.002 (2)
C110.0268 (14)0.0317 (14)0.0372 (15)0.0004 (11)0.0074 (12)0.0104 (12)
C120.0343 (15)0.0351 (15)0.0435 (17)0.0039 (13)0.0076 (13)0.0147 (13)
C130.0429 (17)0.0323 (15)0.0444 (18)0.0009 (13)0.0067 (14)0.0114 (13)
C140.071 (2)0.0411 (18)0.060 (2)0.0028 (17)0.0160 (19)0.0223 (17)
C150.0242 (14)0.0358 (15)0.0474 (17)0.0013 (12)0.0047 (12)0.0137 (13)
C160.0295 (15)0.0358 (15)0.0470 (18)0.0051 (12)0.0013 (13)0.0108 (13)
C170.0400 (18)0.0456 (18)0.056 (2)0.0054 (15)0.0089 (16)0.0127 (16)
C180.072 (3)0.062 (2)0.052 (2)0.010 (2)0.0131 (19)0.0136 (19)
Geometric parameters (Å, º) top
Ni—S1i2.2093 (7)C3—C41.392 (5)
Ni—S12.2093 (7)C4—C51.366 (6)
Ni—P12.2361 (7)C5—C61.375 (5)
Ni—P1i2.2361 (7)C7—C81.518 (4)
Cl—C41.746 (3)C8—C91.524 (5)
S1—C11.749 (3)C9—C101.500 (6)
P1—C71.829 (3)C11—C121.523 (4)
P1—C151.830 (3)C12—C131.526 (4)
P1—C111.835 (3)C13—C141.517 (4)
C1—C21.383 (5)C15—C161.528 (4)
C1—C61.420 (4)C16—C171.527 (4)
C2—C31.385 (4)C17—C181.520 (5)
S1i—Ni—S1180.00 (4)C1—C2—C3121.6 (3)
S1i—Ni—P193.43 (3)C2—C3—C4118.3 (4)
S1—Ni—P186.57 (3)C5—C4—C3121.7 (3)
S1i—Ni—P1i86.57 (3)C5—C4—Cl119.3 (3)
S1—Ni—P1i93.43 (3)C3—C4—Cl119.0 (3)
P1—Ni—P1i180.00 (3)C4—C5—C6120.0 (3)
C1—S1—Ni107.70 (11)C5—C6—C1120.0 (3)
C7—P1—C15103.37 (14)C8—C7—P1113.5 (2)
C7—P1—C11103.70 (14)C7—C8—C9112.4 (3)
C15—P1—C11104.52 (13)C10—C9—C8113.9 (4)
C7—P1—Ni116.13 (10)C12—C11—P1118.0 (2)
C15—P1—Ni108.05 (10)C11—C12—C13111.5 (2)
C11—P1—Ni119.39 (9)C14—C13—C12113.6 (3)
C2—C1—C6118.4 (3)C16—C15—P1113.17 (19)
C2—C1—S1123.9 (2)C17—C16—C15113.0 (3)
C6—C1—S1117.7 (3)C18—C17—C16112.5 (3)
Symmetry code: (i) x+1, y+2, z+2.
 

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