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High-resolution X-ray diffraction experiments, theoretical calculations and atom-specific X-ray absorption experiments were used to investigate two nickel complexes, (MePh3P)2[NiII(bdtCl2)2]·2(CH3)2SO [complex (1)] and (MePh3P)[NiIII(bdtCl2)2] [complex (2)]. Combining the techniques of nickel K- and sulfur K-edge X-ray absorption spectroscopy with high-resolution X-ray charge density modeling, together with theoretical calculations, the actual oxidation states of the central Ni atoms in these two complexes are investigated. Ni ions in two complexes are clearly in different oxidation states: the Ni ion of complex (1) is formally NiII; that of complex (2) should be formally NiIII, yet it is best described as a combination of Ni2+ and Ni3+, due to the involvement of the non-innocent ligand in the Ni—L bond. A detailed description of Ni—S bond character (σ,π) is presented.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520621011495/px5045sup1.cif
Contains datablocks global, 1_100K, 2_100K, 2_15K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520621011495/px50451_100Ksup2.hkl
Contains datablock 1_100K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520621011495/px50452_100Ksup3.hkl
Contains datablock 2_100K

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520621011495/px50452_15Ksup4.hkl
Contains datablock 2_15K

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S2052520621011495/px5045sup5.pdf
Supporting information, including Tables S1-S6 and Figures S1-S8

CCDC references: 2119610; 2122285; 2122286

Computing details top

For all structures, program(s) used to solve structure: ShelXT (Sheldrick, 2015); program(s) used to refine structure: SHELXL (Sheldrick, 2015); molecular graphics: Olex2 (Dolomanov et al., 2009); software used to prepare material for publication: Olex2 (Dolomanov et al., 2009).

(1_100K) top
Crystal data top
C12H4Cl4NiS4·2(C2H6OS)·2(C19H18P)F(000) = 1228
Mr = 1187.76Dx = 1.494 Mg m3
Monoclinic, P21/nAg Kα radiation, λ = 0.56083 Å
a = 13.8788 (1) ÅCell parameters from 564441 reflections
b = 11.5765 (1) Åθ = 2.1–39.7°
c = 16.4387 (1) ŵ = 0.47 mm1
β = 90.651 (1)°T = 100 K
V = 2641.00 (3) Å3Plate, yellow-brown
Z = 20.32 × 0.18 × 0.05 mm
Data collection top
STOE STADIVARI
diffractometer
32089 independent reflections
Radiation source: Incoatec HB Iµs 2.0, Incoatec Ag tube21588 reflections with I > 2σ(I)
Graded multilayer mirror monochromatorRint = 0.046
Detector resolution: 5.81 pixels mm-1θmax = 39.8°, θmin = 2.1°
rotation method, ω scansh = 2931
Absorption correction: integration
STOE X-Red32, absorption correction by Gaussian integration, analogous to P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis", published in F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard, Copenhagen (1970), 255 - 270
k = 2626
Tmin = 0.934, Tmax = 0.985l = 3734
423226 measured reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.033H-atom parameters constrained
wR(F2) = 0.098 w = 1/[σ2(Fo2) + (0.0475P)2 + 0.4625P]
where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.003
32089 reflectionsΔρmax = 1.14 e Å3
316 parametersΔρmin = 0.76 e Å3
0 restraints
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.20021 (4)0.88418 (5)0.52472 (3)0.01313 (7)
C20.13591 (4)0.78907 (5)0.52492 (3)0.01350 (7)
C30.17364 (4)0.67962 (5)0.54380 (3)0.01548 (8)
C40.27071 (4)0.66152 (6)0.56147 (4)0.01772 (9)
H40.2932940.5877430.5734250.021*
C50.33352 (4)0.75489 (6)0.56106 (4)0.01729 (8)
H50.3985980.7446090.5730570.021*
C60.29765 (4)0.86390 (5)0.54244 (3)0.01478 (7)
Cl10.37771 (2)0.98020 (2)0.54315 (2)0.01908 (3)
Cl20.09648 (2)0.56120 (2)0.54697 (2)0.02062 (3)
Ni10.0000001.0000000.5000000.01174 (2)
S10.15530 (2)1.02168 (2)0.50391 (2)0.01428 (2)
S20.01443 (2)0.81311 (2)0.50318 (2)0.01503 (2)
C260.70855 (9)0.57799 (10)0.25536 (7)0.0377 (2)
H26A0.7486420.5455160.2974810.057*
H26B0.6764780.6453250.2757520.057*
H26C0.7476250.5991060.2098950.057*
C270.70375 (7)0.36013 (8)0.20150 (5)0.02960 (15)
H27A0.7493000.3862340.1620130.044*
H27B0.6688110.2950840.1801340.044*
H27C0.7373490.3377840.2503780.044*
O10.56948 (4)0.43752 (6)0.29888 (4)0.02617 (10)
S30.62136 (2)0.47433 (2)0.22379 (2)0.02183 (3)
C70.34485 (5)0.40980 (6)0.20600 (4)0.01922 (9)
H7A0.3415930.4472360.1539380.029*
H7B0.3030280.3437400.2057440.029*
H7C0.4098400.3854080.2168750.029*
C80.18880 (4)0.56026 (5)0.26145 (3)0.01439 (7)
C90.12574 (5)0.59057 (6)0.32376 (4)0.01722 (8)
H90.1432450.5780440.3778180.021*
C100.03684 (5)0.63948 (6)0.30458 (4)0.01891 (9)
H100.0057830.6583720.3457490.023*
C110.01174 (4)0.66011 (6)0.22368 (4)0.01853 (9)
H110.0478020.6926340.2108870.022*
C120.07536 (4)0.63228 (6)0.16178 (4)0.01774 (9)
H120.0585220.6473980.1079050.021*
C130.16383 (4)0.58206 (6)0.18015 (3)0.01644 (8)
H130.2061380.5630610.1387780.020*
C140.38485 (4)0.63244 (5)0.28524 (3)0.01336 (7)
C150.43798 (5)0.66269 (6)0.21702 (4)0.01766 (8)
H150.4373230.6157250.1711210.021*
C160.49209 (5)0.76407 (6)0.21835 (4)0.02141 (10)
H160.5275290.7849900.1729920.026*
C170.49346 (5)0.83402 (6)0.28689 (4)0.02005 (10)
H170.5307710.9007410.2876890.024*
C180.43908 (5)0.80455 (6)0.35449 (4)0.01878 (9)
H180.4394580.8520760.4001110.023*
C190.38426 (5)0.70411 (5)0.35374 (3)0.01654 (8)
H190.3473540.6846300.3985650.020*
C200.31289 (4)0.43517 (5)0.37895 (3)0.01433 (7)
C210.23395 (5)0.37231 (6)0.40719 (5)0.02025 (10)
H210.1761170.3724860.3780500.024*
C220.24239 (5)0.30956 (6)0.47906 (5)0.02388 (12)
H220.1897870.2686760.4985480.029*
C230.32934 (6)0.30788 (6)0.52179 (4)0.02208 (11)
H230.3347560.2657320.5697850.026*
C240.40817 (5)0.36878 (6)0.49318 (4)0.01910 (9)
H240.4662640.3669070.5219120.023*
C250.40059 (4)0.43256 (5)0.42177 (3)0.01563 (8)
H250.4534570.4732260.4025650.019*
P10.30785 (2)0.50825 (2)0.28302 (2)0.01294 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.01217 (15)0.01552 (18)0.01170 (15)0.00044 (13)0.00003 (12)0.00018 (13)
C20.01322 (16)0.01449 (18)0.01282 (16)0.00049 (13)0.00104 (13)0.00047 (13)
C30.01699 (18)0.01457 (18)0.01492 (18)0.00116 (15)0.00207 (15)0.00058 (14)
C40.0186 (2)0.0185 (2)0.01606 (19)0.00494 (17)0.00119 (16)0.00147 (16)
C50.01477 (18)0.0216 (2)0.01543 (19)0.00428 (16)0.00081 (14)0.00021 (16)
C60.01212 (16)0.0188 (2)0.01339 (17)0.00089 (14)0.00016 (13)0.00081 (15)
Cl10.01217 (4)0.02283 (6)0.02221 (6)0.00163 (4)0.00128 (4)0.00260 (5)
Cl20.02347 (6)0.01390 (5)0.02461 (6)0.00095 (4)0.00527 (5)0.00048 (4)
Ni10.01097 (3)0.01294 (3)0.01130 (3)0.00013 (3)0.00028 (2)0.00049 (3)
S10.01211 (4)0.01396 (5)0.01675 (5)0.00063 (4)0.00073 (4)0.00095 (4)
S20.01241 (4)0.01414 (5)0.01853 (5)0.00102 (4)0.00017 (4)0.00048 (4)
C260.0461 (5)0.0327 (4)0.0346 (4)0.0137 (4)0.0114 (4)0.0004 (3)
C270.0324 (4)0.0286 (4)0.0280 (3)0.0110 (3)0.0074 (3)0.0031 (3)
O10.0229 (2)0.0295 (3)0.0263 (2)0.00218 (19)0.00738 (18)0.0043 (2)
S30.02443 (7)0.02297 (7)0.01815 (6)0.00590 (6)0.00238 (5)0.00205 (5)
C70.0228 (2)0.0166 (2)0.0181 (2)0.00303 (18)0.00245 (18)0.00430 (17)
C80.01524 (17)0.01426 (18)0.01360 (17)0.00042 (14)0.00283 (13)0.00025 (14)
C90.0190 (2)0.0183 (2)0.01426 (18)0.00229 (16)0.00122 (15)0.00028 (15)
C100.0193 (2)0.0188 (2)0.0187 (2)0.00295 (17)0.00007 (17)0.00073 (17)
C110.01683 (19)0.0176 (2)0.0211 (2)0.00211 (16)0.00277 (17)0.00089 (17)
C120.01733 (19)0.0195 (2)0.01633 (19)0.00114 (16)0.00403 (15)0.00216 (16)
C130.01614 (18)0.0191 (2)0.01403 (18)0.00058 (16)0.00239 (14)0.00083 (15)
C140.01527 (17)0.01253 (17)0.01226 (16)0.00013 (13)0.00095 (13)0.00035 (13)
C150.0225 (2)0.0164 (2)0.01415 (18)0.00095 (17)0.00306 (16)0.00018 (15)
C160.0267 (3)0.0183 (2)0.0193 (2)0.0033 (2)0.0063 (2)0.00177 (18)
C170.0234 (2)0.0145 (2)0.0223 (2)0.00298 (18)0.00232 (19)0.00092 (17)
C180.0242 (2)0.0147 (2)0.0175 (2)0.00266 (17)0.00067 (18)0.00214 (16)
C190.0210 (2)0.01515 (19)0.01351 (17)0.00224 (16)0.00148 (15)0.00133 (14)
C200.01564 (17)0.01261 (17)0.01469 (17)0.00110 (14)0.00180 (14)0.00163 (14)
C210.0173 (2)0.0155 (2)0.0279 (3)0.00356 (16)0.00173 (19)0.00446 (19)
C220.0233 (3)0.0169 (2)0.0316 (3)0.00259 (19)0.0053 (2)0.0079 (2)
C230.0291 (3)0.0179 (2)0.0194 (2)0.0019 (2)0.0038 (2)0.00657 (18)
C240.0226 (2)0.0192 (2)0.01544 (19)0.00185 (18)0.00252 (17)0.00348 (17)
C250.01590 (18)0.01669 (19)0.01426 (17)0.00084 (15)0.00139 (14)0.00235 (15)
P10.01473 (5)0.01206 (5)0.01198 (5)0.00037 (4)0.00260 (4)0.00037 (4)
Geometric parameters (Å, º) top
C1—C21.4173 (8)C8—P11.7903 (6)
C1—C61.4000 (7)C9—C101.3906 (9)
C1—S11.7419 (6)C10—C111.3916 (9)
C2—C31.4044 (8)C11—C121.3925 (9)
C2—S21.7418 (5)C12—C131.3887 (8)
C3—C41.3909 (8)C14—C151.3938 (8)
C3—Cl21.7407 (6)C14—C191.3988 (8)
C4—C51.3886 (10)C14—P11.7915 (6)
C5—C61.3894 (9)C15—C161.3933 (9)
C6—Cl11.7456 (6)C16—C171.3874 (10)
Ni1—S12.1702 (1)C17—C181.3929 (9)
Ni1—S1i2.1702 (1)C18—C191.3895 (9)
Ni1—S2i2.1733 (2)C20—C211.3988 (8)
Ni1—S22.1733 (2)C20—C251.3996 (8)
C26—S31.7775 (11)C20—P11.7903 (6)
C27—S31.7885 (8)C21—C221.3908 (10)
O1—S31.4980 (6)C22—C231.3895 (11)
C7—P11.7833 (6)C23—C241.3881 (10)
C8—C91.3994 (8)C24—C251.3897 (8)
C8—C131.3998 (8)
C2—C1—S1119.10 (4)C10—C9—C8119.79 (5)
C6—C1—C2118.42 (5)C9—C10—C11119.89 (6)
C6—C1—S1122.47 (4)C10—C11—C12120.31 (6)
C1—C2—S2118.91 (4)C13—C12—C11120.29 (5)
C3—C2—C1117.92 (5)C12—C13—C8119.46 (5)
C3—C2—S2123.17 (4)C15—C14—C19120.44 (5)
C2—C3—Cl2119.29 (4)C15—C14—P1120.40 (4)
C4—C3—C2122.68 (6)C19—C14—P1118.92 (4)
C4—C3—Cl2118.02 (5)C16—C15—C14119.27 (6)
C5—C4—C3119.23 (6)C17—C16—C15120.45 (6)
C4—C5—C6119.00 (5)C16—C17—C18120.17 (6)
C1—C6—Cl1119.03 (5)C19—C18—C17119.95 (6)
C5—C6—C1122.75 (6)C18—C19—C14119.70 (5)
C5—C6—Cl1118.21 (4)C21—C20—C25120.12 (5)
S1—Ni1—S1i180.0C21—C20—P1121.01 (5)
S1i—Ni1—S288.673 (5)C25—C20—P1118.57 (4)
S1i—Ni1—S2i91.326 (5)C22—C21—C20119.66 (6)
S1—Ni1—S291.326 (5)C23—C22—C21120.07 (6)
S1—Ni1—S2i88.674 (5)C24—C23—C22120.33 (6)
S2i—Ni1—S2180.0C23—C24—C25120.24 (6)
C1—S1—Ni1104.669 (18)C24—C25—C20119.56 (5)
C2—S2—Ni1104.64 (2)C7—P1—C8110.30 (3)
C26—S3—C2797.13 (5)C7—P1—C14110.54 (3)
O1—S3—C26106.47 (4)C7—P1—C20108.34 (3)
O1—S3—C27105.84 (4)C8—P1—C14106.45 (3)
C9—C8—C13120.23 (5)C8—P1—C20111.10 (3)
C9—C8—P1121.52 (4)C20—P1—C14110.12 (3)
C13—C8—P1117.88 (4)
Symmetry code: (i) x, y+2, z+1.
(2_100K) top
Crystal data top
2(C6H2Cl2Ni0.5S2)·C19H18PF(000) = 1532
Mr = 754.20Dx = 1.622 Mg m3
Monoclinic, P21/cAg Kα radiation, λ = 0.56083 Å
a = 13.3664 (1) ÅCell parameters from 1181142 reflections
b = 14.4849 (1) Åθ = 2.0–39.2°
c = 15.9712 (1) ŵ = 0.68 mm1
β = 93.054 (1)°T = 100 K
V = 3087.81 (4) Å3Plate, black-green
Z = 40.23 × 0.16 × 0.03 mm
Data collection top
STOE STADIVARI
diffractometer
36081 independent reflections
Radiation source: Incoatec HB Iµs 2.0, Incoatec Ag tube25847 reflections with I > 2σ(I)
Graded multilayer mirror monochromatorRint = 0.030
Detector resolution: 5.81 pixels mm-1θmax = 39.2°, θmin = 2.0°
rotation method, ω scansh = 2929
Absorption correction: multi-scan
STOE X-Red32, absorption correction by Gaussian integration, analogous to P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different absorption corrections on the model structure of tetrakis(µ2-acetato)- diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140. Finally a spherical absorption correction was done within STOE LANA.
k = 3229
Tmin = 0.262, Tmax = 0.834l = 3435
653883 measured reflections
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.026H-atom parameters constrained
wR(F2) = 0.079 w = 1/[σ2(Fo2) + (0.0343P)2 + 0.6067P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.006
36081 reflectionsΔρmax = 0.83 e Å3
375 parametersΔρmin = 0.74 e Å3
0 restraints
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.5000000.5000001.0000000.01386 (1)
Cl10.44153 (2)0.15548 (2)1.08435 (2)0.02660 (3)
Cl20.11275 (2)0.44048 (2)0.97156 (2)0.02688 (3)
S10.50447 (2)0.35367 (2)1.02194 (2)0.01689 (2)
S20.33996 (2)0.50270 (2)0.99057 (2)0.01750 (2)
C10.37965 (4)0.32298 (4)1.02682 (3)0.01685 (7)
C20.34982 (5)0.23424 (4)1.05051 (4)0.02083 (9)
C30.24999 (6)0.20960 (5)1.05044 (4)0.02665 (12)
H30.2318810.1506921.0671510.032*
C40.17663 (5)0.27349 (5)1.02520 (4)0.02646 (12)
H40.1094090.2566151.0227230.032*
C50.20406 (4)0.36210 (5)1.00384 (4)0.02089 (9)
C60.30501 (4)0.38957 (4)1.00741 (3)0.01693 (7)
Ni20.0000000.5000000.5000000.01217 (1)
Cl30.05222 (2)0.57008 (2)0.81887 (2)0.02373 (3)
Cl40.13497 (2)0.83647 (2)0.56430 (2)0.02342 (3)
S30.03683 (2)0.50657 (2)0.62876 (2)0.01552 (2)
S40.06282 (2)0.63643 (2)0.50385 (2)0.01479 (2)
C70.00302 (4)0.61503 (4)0.66256 (3)0.01500 (6)
C80.00609 (4)0.64505 (4)0.74573 (3)0.01812 (8)
C90.02238 (5)0.73304 (5)0.77058 (4)0.02198 (9)
H90.0140030.7522790.8253170.026*
C100.06366 (5)0.79287 (4)0.71342 (4)0.02200 (9)
H100.0818290.8524790.7296270.026*
C110.07750 (4)0.76330 (4)0.63253 (4)0.01800 (8)
C120.04696 (4)0.67476 (4)0.60532 (3)0.01490 (6)
P10.38094 (2)0.11135 (2)1.18222 (2)0.01378 (2)
C130.33689 (5)0.12594 (5)1.07500 (4)0.02218 (10)
H13A0.3684690.1789691.0518510.033*
H13B0.3530320.0720151.0434830.033*
H13C0.2655900.1346351.0722790.033*
C140.33966 (4)0.20663 (3)1.24227 (3)0.01549 (7)
C150.29695 (4)0.19089 (4)1.31877 (3)0.01739 (7)
H150.2900910.1309821.3386240.021*
C160.26466 (5)0.26544 (4)1.36519 (4)0.02086 (9)
H160.2360110.2555521.4162330.025*
C170.27529 (5)0.35440 (4)1.33518 (5)0.02442 (11)
H170.2531150.4040801.3660850.029*
C180.31882 (5)0.37023 (4)1.25928 (5)0.02614 (12)
H180.3260810.4303011.2399550.031*
C190.35142 (5)0.29653 (4)1.21235 (4)0.02137 (9)
H190.3807110.3067831.1616430.026*
C200.51456 (3)0.10846 (4)1.18638 (3)0.01423 (6)
C210.56463 (4)0.07975 (4)1.11644 (3)0.01693 (7)
H210.5285310.0597511.0684420.020*
C220.66841 (4)0.08122 (4)1.11888 (3)0.01796 (8)
H220.7020690.0639341.0718700.022*
C230.72213 (4)0.10845 (4)1.19143 (4)0.01783 (7)
H230.7917770.1089351.1929660.021*
C240.67249 (4)0.13499 (4)1.26180 (4)0.01928 (8)
H240.7089630.1519451.3106020.023*
C250.56850 (4)0.13623 (4)1.25937 (3)0.01774 (8)
H250.5350650.1553911.3059220.021*
C260.33116 (4)0.00789 (3)1.22352 (3)0.01579 (7)
C270.22827 (4)0.00801 (4)1.21151 (5)0.02242 (10)
H270.1882540.0331741.1801050.027*
C280.18611 (5)0.08534 (5)1.24655 (5)0.02560 (11)
H280.1175790.0958981.2391380.031*
C290.24644 (5)0.14719 (4)1.29284 (4)0.02289 (10)
H290.2180480.1990891.3163200.027*
C300.34841 (5)0.13191 (4)1.30413 (4)0.02172 (9)
H300.3883560.1739611.3345790.026*
C310.39149 (4)0.05398 (4)1.27017 (4)0.01834 (8)
H310.4598870.0432241.2784890.022*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.01229 (3)0.01431 (3)0.01497 (3)0.00180 (2)0.00053 (2)0.00185 (3)
Cl10.04480 (9)0.01647 (5)0.01878 (5)0.00133 (5)0.00394 (5)0.00278 (4)
Cl20.01391 (5)0.03989 (9)0.02695 (6)0.00238 (5)0.00203 (4)0.00594 (6)
S10.01661 (5)0.01574 (5)0.01825 (5)0.00083 (4)0.00039 (4)0.00264 (4)
S20.01315 (4)0.01774 (5)0.02160 (5)0.00104 (4)0.00098 (4)0.00140 (4)
C10.01978 (18)0.01683 (17)0.01413 (15)0.00465 (14)0.00279 (13)0.00000 (13)
C20.0299 (3)0.01710 (19)0.01605 (17)0.00653 (17)0.00611 (17)0.00146 (15)
C30.0347 (3)0.0227 (2)0.0236 (2)0.0142 (2)0.0116 (2)0.00559 (19)
C40.0246 (2)0.0307 (3)0.0250 (2)0.0147 (2)0.0094 (2)0.0084 (2)
C50.01665 (18)0.0280 (2)0.01835 (19)0.00734 (17)0.00420 (15)0.00556 (18)
C60.01554 (16)0.01981 (19)0.01562 (16)0.00484 (14)0.00262 (13)0.00138 (14)
Ni20.01024 (3)0.01420 (3)0.01220 (3)0.00101 (2)0.00178 (2)0.00023 (2)
Cl30.02453 (6)0.03282 (7)0.01415 (4)0.00243 (5)0.00392 (4)0.00092 (4)
Cl40.02408 (6)0.01630 (5)0.03000 (7)0.00139 (4)0.00243 (5)0.00118 (4)
S30.01530 (4)0.01794 (5)0.01360 (4)0.00096 (3)0.00338 (3)0.00016 (3)
S40.01415 (4)0.01528 (4)0.01515 (4)0.00025 (3)0.00261 (3)0.00088 (3)
C70.01235 (14)0.01852 (17)0.01420 (15)0.00230 (12)0.00126 (11)0.00099 (13)
C80.01555 (16)0.0240 (2)0.01486 (16)0.00296 (15)0.00112 (13)0.00222 (15)
C90.0200 (2)0.0263 (2)0.0195 (2)0.00289 (18)0.00020 (16)0.00742 (18)
C100.0202 (2)0.0208 (2)0.0248 (2)0.00172 (17)0.00049 (17)0.00694 (18)
C110.01578 (16)0.01621 (17)0.0219 (2)0.00141 (13)0.00032 (14)0.00188 (15)
C120.01241 (14)0.01575 (16)0.01652 (16)0.00195 (12)0.00083 (12)0.00071 (13)
P10.01149 (4)0.01543 (5)0.01436 (4)0.00148 (3)0.00019 (3)0.00147 (4)
C130.01776 (19)0.0317 (3)0.01672 (18)0.00233 (18)0.00282 (15)0.00045 (18)
C140.01375 (15)0.01417 (15)0.01864 (17)0.00182 (12)0.00179 (13)0.00105 (13)
C150.01764 (17)0.01682 (17)0.01784 (17)0.00248 (14)0.00204 (14)0.00150 (14)
C160.0195 (2)0.0210 (2)0.0223 (2)0.00179 (16)0.00343 (16)0.00575 (17)
C170.0203 (2)0.0179 (2)0.0354 (3)0.00084 (16)0.0048 (2)0.0087 (2)
C180.0245 (2)0.01407 (18)0.0405 (4)0.00009 (17)0.0078 (2)0.0017 (2)
C190.0207 (2)0.01561 (18)0.0283 (2)0.00043 (15)0.00625 (18)0.00154 (17)
C200.01211 (13)0.01671 (16)0.01390 (14)0.00113 (12)0.00105 (11)0.00122 (12)
C210.01548 (16)0.0218 (2)0.01361 (15)0.00187 (14)0.00165 (13)0.00148 (14)
C220.01594 (17)0.0210 (2)0.01738 (17)0.00275 (14)0.00478 (14)0.00074 (15)
C230.01293 (15)0.01821 (18)0.0225 (2)0.00043 (13)0.00255 (14)0.00026 (16)
C240.01362 (16)0.0235 (2)0.02051 (19)0.00008 (15)0.00093 (14)0.00540 (17)
C250.01391 (15)0.0233 (2)0.01594 (16)0.00078 (14)0.00063 (13)0.00529 (15)
C260.01372 (15)0.01444 (16)0.01922 (18)0.00139 (12)0.00107 (13)0.00238 (13)
C270.01422 (17)0.01721 (19)0.0356 (3)0.00002 (14)0.00031 (18)0.00130 (19)
C280.0186 (2)0.0190 (2)0.0394 (3)0.00301 (17)0.0029 (2)0.0001 (2)
C290.0266 (2)0.01672 (19)0.0259 (2)0.00165 (17)0.0061 (2)0.00134 (18)
C300.0257 (2)0.0195 (2)0.0201 (2)0.00256 (18)0.00197 (18)0.00141 (17)
C310.01761 (18)0.01937 (19)0.01799 (18)0.00242 (15)0.00044 (14)0.00024 (15)
Geometric parameters (Å, º) top
Ni1—S12.1486 (1)C13—H13A0.9600
Ni1—S1i2.1487 (1)C13—H13B0.9600
Ni1—S22.1369 (1)C13—H13C0.9600
Ni1—S2i2.1369 (1)C14—C151.3947 (8)
Cl1—C21.7394 (7)C14—C191.3989 (8)
Cl2—C51.7254 (7)C15—H150.9300
S1—C11.7323 (6)C15—C161.3914 (8)
S2—C61.7290 (6)C16—H160.9300
C1—C21.4038 (8)C16—C171.3848 (10)
C1—C61.4102 (8)C17—H170.9300
C2—C31.3812 (10)C17—C181.3914 (11)
C3—H30.9300C18—H180.9300
C3—C41.3921 (12)C18—C191.3878 (9)
C4—H40.9300C19—H190.9300
C4—C51.3826 (10)C20—C211.3958 (7)
C5—C61.4051 (7)C20—C251.3968 (7)
Ni2—S32.1420 (1)C21—H210.9300
Ni2—S3ii2.1421 (1)C21—C221.3858 (8)
Ni2—S4ii2.1467 (1)C22—H220.9300
Ni2—S42.1467 (1)C22—C231.3874 (8)
Cl3—C81.7322 (6)C23—H230.9300
Cl4—C111.7292 (6)C23—C241.3895 (8)
S3—C71.7357 (6)C24—H240.9300
S4—C121.7367 (5)C24—C251.3885 (7)
C7—C81.4091 (7)C25—H250.9300
C7—C121.4094 (7)C26—C271.3975 (8)
C8—C91.3823 (9)C26—C311.3945 (8)
C9—H90.9300C27—H270.9300
C9—C101.3937 (10)C27—C281.3853 (9)
C10—H100.9300C28—H280.9300
C10—C111.3827 (9)C28—C291.3915 (10)
C11—C121.4076 (7)C29—H290.9300
P1—C131.7934 (6)C29—C301.3831 (10)
P1—C141.7847 (5)C30—H300.9300
P1—C201.7843 (5)C30—C311.3903 (9)
P1—C261.7806 (6)C31—H310.9300
S1—Ni1—S1i180.0P1—C13—H13B109.5
S2i—Ni1—S187.216 (5)P1—C13—H13C109.5
S2—Ni1—S1i87.216 (5)H13A—C13—H13B109.5
S2i—Ni1—S1i92.784 (5)H13A—C13—H13C109.5
S2—Ni1—S192.784 (5)H13B—C13—H13C109.5
S2—Ni1—S2i180.0C15—C14—P1119.81 (4)
C1—S1—Ni1104.00 (2)C15—C14—C19120.68 (5)
C6—S2—Ni1104.443 (19)C19—C14—P1119.52 (4)
C2—C1—S1122.35 (5)C14—C15—H15120.2
C2—C1—C6118.54 (5)C16—C15—C14119.53 (5)
C6—C1—S1119.10 (4)C16—C15—H15120.2
C1—C2—Cl1118.60 (5)C15—C16—H16120.1
C3—C2—Cl1119.71 (5)C17—C16—C15119.82 (6)
C3—C2—C1121.64 (7)C17—C16—H16120.1
C2—C3—H3120.2C16—C17—H17119.7
C2—C3—C4119.61 (6)C16—C17—C18120.69 (6)
C4—C3—H3120.2C18—C17—H17119.7
C3—C4—H4120.1C17—C18—H18119.9
C5—C4—C3119.78 (6)C19—C18—C17120.11 (6)
C5—C4—H4120.1C19—C18—H18119.9
C4—C5—Cl2119.47 (5)C14—C19—H19120.4
C4—C5—C6121.30 (7)C18—C19—C14119.16 (6)
C6—C5—Cl2119.23 (5)C18—C19—H19120.4
C1—C6—S2119.25 (4)C21—C20—P1119.93 (4)
C5—C6—S2121.93 (5)C21—C20—C25120.37 (4)
C5—C6—C1118.81 (5)C25—C20—P1119.70 (4)
S3—Ni2—S3ii180.0C20—C21—H21120.2
S3—Ni2—S4ii87.645 (5)C22—C21—C20119.65 (5)
S3ii—Ni2—S4ii92.355 (5)C22—C21—H21120.2
S3—Ni2—S492.357 (5)C21—C22—H22120.0
S3ii—Ni2—S487.643 (5)C21—C22—C23120.04 (5)
S4ii—Ni2—S4180.0C23—C22—H22120.0
C7—S3—Ni2104.856 (18)C22—C23—H23119.8
C12—S4—Ni2104.718 (18)C22—C23—C24120.40 (5)
C8—C7—S3122.14 (4)C24—C23—H23119.8
C8—C7—C12118.82 (5)C23—C24—H24120.0
C12—C7—S3119.04 (4)C25—C24—C23120.09 (5)
C7—C8—Cl3119.61 (5)C25—C24—H24120.0
C9—C8—Cl3119.13 (4)C20—C25—H25120.3
C9—C8—C7121.25 (6)C24—C25—C20119.41 (5)
C8—C9—H9120.1C24—C25—H25120.3
C8—C9—C10119.85 (5)C27—C26—P1118.18 (4)
C10—C9—H9120.1C31—C26—P1121.47 (4)
C9—C10—H10120.1C31—C26—C27120.28 (5)
C11—C10—C9119.78 (6)C26—C27—H27120.1
C11—C10—H10120.1C28—C27—C26119.76 (6)
C10—C11—Cl4119.01 (5)C28—C27—H27120.1
C10—C11—C12121.31 (6)C27—C28—H28120.0
C12—C11—Cl4119.68 (4)C27—C28—C29119.91 (6)
C7—C12—S4119.00 (4)C29—C28—H28120.0
C11—C12—S4122.12 (4)C28—C29—H29119.8
C11—C12—C7118.88 (5)C30—C29—C28120.36 (6)
C14—P1—C13109.08 (3)C30—C29—H29119.8
C20—P1—C13108.38 (3)C29—C30—H30119.8
C20—P1—C14109.61 (2)C29—C30—C31120.32 (6)
C26—P1—C13110.04 (3)C31—C30—H30119.8
C26—P1—C14108.63 (3)C26—C31—H31120.3
C26—P1—C20111.07 (2)C30—C31—C26119.37 (5)
P1—C13—H13A109.5C30—C31—H31120.3
Symmetry codes: (i) x+1, y+1, z+2; (ii) x, y+1, z+1.
(2_15K) top
Crystal data top
2(C6H2Cl2Ni0.5S2)·C19H18PF(000) = 1532
Mr = 754.20Dx = 1.628 Mg m3
Monoclinic, P21/cSynchrotron radiation, λ = 0.30996 Å
a = 13.3785 (1) ÅCell parameters from 590779 reflections
b = 14.4463 (2) Åθ = 1.5–28.0°
c = 15.9474 (2) ŵ = 1.33 mm1
β = 93.364 (1)°T = 15 K
V = 3076.84 (6) Å3Plate, black-green
Z = 40.09 × 0.05 × 0.03 mm
Data collection top
Bruker D8 goniometer
diffractometer
89538 independent reflections
Radiation source: synchrotron, Incoatec Iµs64088 reflections with I > 2σ(I)
Mirror optics monochromatorRint = 0.050
ω and phi scansθmax = 28.0°, θmin = 1.5°
Absorption correction: multi-scan
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0490 before and 0.0490 after correction. The Ratio of minimum to maximum transmission is 0.8937. The λ/2 correction factor is Not present.
h = 3740
Tmin = 0.894, Tmax = 1.000k = 4243
831499 measured reflectionsl = 4648
Refinement top
Refinement on F2Primary atom site location: dual
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.032H-atom parameters constrained
wR(F2) = 0.085 w = 1/[σ2(Fo2) + (0.0408P)2 + 0.1535P]
where P = (Fo2 + 2Fc2)/3
S = 1.03(Δ/σ)max = 0.010
88732 reflectionsΔρmax = 2.47 e Å3
374 parametersΔρmin = 3.18 e Å3
0 restraints
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.5000000.5000001.0000000.00407 (1)
Cl10.44448 (2)0.15373 (2)1.08440 (2)0.00792 (1)
Cl20.11211 (2)0.43810 (2)0.97214 (2)0.00817 (1)
S10.50536 (2)0.35281 (2)1.02086 (2)0.00548 (1)
S20.33962 (2)0.50202 (2)0.99069 (2)0.00584 (1)
C10.38065 (2)0.32154 (2)1.02661 (2)0.00575 (2)
C20.35180 (2)0.23228 (2)1.05090 (2)0.00678 (3)
C30.25192 (2)0.20695 (2)1.05173 (2)0.00856 (3)
H30.2344700.1478991.0689080.010*
C40.17752 (2)0.27093 (2)1.02652 (2)0.00860 (3)
H40.1104370.2537411.0245180.010*
C50.20428 (2)0.36009 (2)1.00453 (2)0.00686 (3)
C60.30529 (2)0.38815 (2)1.00754 (2)0.00586 (2)
Ni20.0000000.5000000.5000000.00379 (1)
Cl30.05100 (2)0.57221 (2)0.81961 (2)0.00734 (1)
Cl40.13695 (2)0.83784 (2)0.56358 (2)0.00749 (1)
S30.03717 (2)0.50762 (2)0.62890 (2)0.00524 (1)
S40.06347 (2)0.63685 (2)0.50351 (2)0.00505 (1)
C70.04762 (2)0.67609 (2)0.60498 (2)0.00541 (2)
C80.07873 (2)0.76507 (2)0.63193 (2)0.00622 (3)
C90.06499 (2)0.79535 (2)0.71291 (2)0.00742 (3)
H90.0832440.8552020.7288780.009*
C100.02350 (2)0.73551 (2)0.77062 (2)0.00744 (3)
H100.0153200.7550740.8253520.009*
C110.00531 (2)0.64699 (2)0.74582 (2)0.00615 (3)
C120.00336 (2)0.61652 (2)0.66255 (2)0.00535 (2)
P130.61912 (2)0.11033 (2)0.81707 (2)0.00417 (1)
C130.66347 (2)0.12491 (2)0.92477 (2)0.00849 (3)
H13A0.7348430.1327380.9277800.013*
H13B0.6465540.0712030.9564380.013*
H13C0.6326970.1785900.9476580.013*
C140.66009 (2)0.20604 (2)0.75689 (2)0.00562 (2)
C150.70290 (2)0.19020 (2)0.68028 (2)0.00666 (3)
H150.7098490.1301330.6604620.008*
C160.73507 (2)0.26509 (2)0.63389 (2)0.00772 (3)
H160.7637100.2551680.5829060.009*
C170.72428 (2)0.35477 (2)0.66392 (2)0.00842 (3)
H170.7464450.4045770.6330640.010*
C180.68044 (2)0.37067 (2)0.74005 (2)0.00883 (3)
H180.6729390.4308800.7593320.011*
C190.64806 (2)0.29652 (2)0.78694 (2)0.00749 (3)
H190.6187810.3066910.8376050.009*
C200.66943 (2)0.00662 (2)0.77580 (2)0.00574 (2)
C210.77294 (2)0.00811 (2)0.78735 (2)0.00794 (3)
H210.8128110.0336860.8185070.010*
C220.81564 (2)0.08552 (2)0.75200 (2)0.00894 (3)
H220.8843320.0953230.7589230.011*
C230.75521 (2)0.14851 (2)0.70608 (2)0.00824 (3)
H230.7838740.2002850.6825010.010*
C240.65227 (2)0.13436 (2)0.69533 (2)0.00790 (3)
H240.6124020.1771060.6653150.009*
C250.60888 (2)0.05629 (2)0.72946 (2)0.00686 (3)
H250.5403420.0461010.7215110.008*
C260.48528 (2)0.10731 (2)0.81253 (2)0.00526 (2)
C270.43547 (2)0.07903 (2)0.88295 (2)0.00651 (3)
H270.4717830.0589750.9310700.008*
C280.33140 (2)0.08107 (2)0.88058 (2)0.00686 (3)
H280.2979670.0640650.9277190.008*
C290.27730 (2)0.10860 (2)0.80754 (2)0.00695 (3)
H290.2077160.1096320.8060670.008*
C300.32663 (2)0.13462 (2)0.73662 (2)0.00730 (3)
H300.2899370.1515800.6876890.009*
C310.43094 (2)0.13522 (2)0.73905 (2)0.00674 (3)
H310.4641800.1539580.6923340.008*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.00351 (1)0.00403 (1)0.00466 (1)0.00053 (1)0.00013 (1)0.00057 (1)
Cl10.01165 (2)0.00550 (2)0.00665 (2)0.00024 (2)0.00098 (2)0.00092 (1)
Cl20.00502 (2)0.01054 (2)0.00893 (2)0.00001 (2)0.00021 (1)0.00047 (2)
S10.00488 (2)0.00489 (2)0.00665 (2)0.00021 (1)0.00025 (1)0.00087 (1)
S20.00427 (2)0.00538 (2)0.00786 (2)0.00030 (1)0.00019 (1)0.00090 (1)
C10.00594 (6)0.00544 (6)0.00590 (6)0.00113 (5)0.00055 (5)0.00039 (5)
C20.00836 (7)0.00552 (6)0.00657 (6)0.00145 (5)0.00146 (5)0.00008 (5)
C30.00945 (8)0.00715 (7)0.00930 (7)0.00312 (6)0.00245 (6)0.00048 (6)
C40.00732 (7)0.00878 (7)0.00987 (8)0.00328 (6)0.00184 (6)0.00101 (6)
C50.00525 (6)0.00796 (7)0.00740 (6)0.00157 (5)0.00068 (5)0.00058 (5)
C60.00502 (6)0.00614 (6)0.00644 (6)0.00107 (5)0.00039 (5)0.00031 (5)
Ni20.00385 (1)0.00406 (1)0.00350 (1)0.00000 (1)0.00060 (1)0.00027 (1)
Cl30.00823 (2)0.00906 (2)0.00486 (2)0.00011 (2)0.00137 (1)0.00050 (1)
Cl40.00864 (2)0.00571 (2)0.00823 (2)0.00093 (1)0.00135 (2)0.00048 (1)
S30.00608 (2)0.00534 (2)0.00440 (2)0.00081 (1)0.00120 (1)0.00034 (1)
S40.00578 (2)0.00493 (2)0.00454 (2)0.00042 (1)0.00107 (1)0.00015 (1)
C70.00584 (6)0.00532 (6)0.00512 (5)0.00009 (5)0.00073 (5)0.00038 (4)
C80.00683 (6)0.00545 (6)0.00641 (6)0.00034 (5)0.00068 (5)0.00057 (5)
C90.00856 (7)0.00647 (6)0.00723 (6)0.00037 (6)0.00059 (6)0.00185 (5)
C100.00855 (7)0.00775 (7)0.00605 (6)0.00018 (6)0.00076 (5)0.00187 (5)
C110.00657 (6)0.00700 (6)0.00495 (5)0.00005 (5)0.00074 (5)0.00069 (5)
C120.00567 (6)0.00573 (6)0.00470 (5)0.00012 (5)0.00080 (5)0.00044 (4)
P130.00375 (2)0.00426 (2)0.00449 (2)0.00027 (1)0.00016 (1)0.00032 (1)
C130.00783 (7)0.01123 (8)0.00623 (6)0.00066 (6)0.00108 (6)0.00009 (6)
C140.00598 (6)0.00473 (5)0.00623 (6)0.00051 (5)0.00108 (5)0.00018 (5)
C150.00797 (7)0.00574 (6)0.00639 (6)0.00059 (5)0.00151 (5)0.00002 (5)
C160.00870 (7)0.00728 (7)0.00738 (7)0.00043 (6)0.00202 (6)0.00128 (5)
C170.00886 (8)0.00616 (6)0.01043 (8)0.00026 (6)0.00228 (6)0.00216 (6)
C180.01031 (8)0.00497 (6)0.01148 (8)0.00025 (6)0.00298 (7)0.00031 (6)
C190.00899 (7)0.00523 (6)0.00851 (7)0.00012 (5)0.00260 (6)0.00037 (5)
C200.00504 (6)0.00482 (6)0.00735 (6)0.00005 (5)0.00028 (5)0.00010 (5)
C210.00551 (6)0.00646 (7)0.01176 (8)0.00024 (5)0.00026 (6)0.00154 (6)
C220.00655 (7)0.00725 (7)0.01300 (9)0.00133 (6)0.00040 (6)0.00128 (6)
C230.00895 (8)0.00621 (6)0.00964 (8)0.00094 (6)0.00135 (6)0.00066 (6)
C240.00872 (7)0.00674 (7)0.00822 (7)0.00054 (6)0.00024 (6)0.00159 (5)
C250.00622 (6)0.00664 (6)0.00767 (6)0.00043 (5)0.00009 (5)0.00080 (5)
C260.00435 (5)0.00634 (6)0.00509 (5)0.00018 (5)0.00027 (4)0.00058 (5)
C270.00576 (6)0.00860 (7)0.00521 (6)0.00037 (5)0.00058 (5)0.00084 (5)
C280.00595 (6)0.00848 (7)0.00628 (6)0.00063 (5)0.00157 (5)0.00019 (5)
C290.00507 (6)0.00789 (7)0.00792 (7)0.00012 (5)0.00061 (5)0.00027 (5)
C300.00549 (6)0.00922 (7)0.00710 (6)0.00014 (6)0.00037 (5)0.00181 (6)
C310.00536 (6)0.00896 (7)0.00590 (6)0.00018 (5)0.00029 (5)0.00183 (5)
Geometric parameters (Å, º) top
Ni1—S1i2.1528 (1)C13—H13A0.9600
Ni1—S12.1528 (1)C13—H13B0.9600
Ni1—S2i2.1423 (1)C13—H13C0.9600
Ni1—S22.1423 (1)C14—C151.3982 (4)
Cl1—C21.7415 (3)C14—C191.4047 (4)
Cl2—C51.7270 (3)C15—H150.9300
S1—C11.7361 (3)C15—C161.3930 (4)
S2—C61.7332 (3)C16—H160.9300
C1—C21.4068 (4)C16—C171.3917 (4)
C1—C61.4139 (4)C17—H170.9300
C2—C31.3862 (4)C17—C181.3979 (4)
C3—H30.9300C18—H180.9300
C3—C41.3999 (5)C18—C191.3901 (4)
C4—H40.9300C19—H190.9300
C4—C51.3873 (4)C20—C211.4026 (4)
C5—C61.4090 (4)C20—C251.3992 (4)
Ni2—S3ii2.1458 (1)C21—H210.9300
Ni2—S32.1459 (1)C21—C221.3902 (4)
Ni2—S4ii2.1510 (1)C22—H220.9300
Ni2—S42.1510 (1)C22—C231.3958 (4)
Cl3—C111.7349 (3)C23—H230.9300
Cl4—C81.7320 (3)C23—C241.3929 (4)
S3—C121.7387 (3)C24—H240.9300
S4—C71.7392 (2)C24—C251.3936 (4)
C7—C81.4104 (3)C25—H250.9300
C7—C121.4135 (3)C26—C271.4001 (3)
C8—C91.3858 (4)C26—C311.4015 (4)
C9—H90.9300C27—H270.9300
C9—C101.4009 (4)C27—C281.3910 (4)
C10—H100.9300C28—H280.9300
C10—C111.3865 (4)C28—C291.3928 (4)
C11—C121.4101 (3)C29—H290.9300
P13—C131.7963 (3)C29—C301.3941 (4)
P13—C141.7875 (3)C30—H300.9300
P13—C201.7840 (3)C30—C311.3938 (4)
P13—C261.7883 (2)C31—H310.9300
S1i—Ni1—S1180.0P13—C13—H13B109.5
S2—Ni1—S192.772 (3)P13—C13—H13C109.5
S2i—Ni1—S1i92.774 (3)H13A—C13—H13B109.5
S2—Ni1—S1i87.227 (3)H13A—C13—H13C109.5
S2i—Ni1—S187.227 (3)H13B—C13—H13C109.5
S2i—Ni1—S2180.0C15—C14—P13119.784 (19)
C1—S1—Ni1103.988 (9)C15—C14—C19120.76 (2)
C6—S2—Ni1104.462 (9)C19—C14—P13119.455 (19)
C2—C1—S1122.22 (2)C14—C15—H15120.3
C2—C1—C6118.64 (2)C16—C15—C14119.48 (2)
C6—C1—S1119.142 (18)C16—C15—H15120.3
C1—C2—Cl1118.67 (2)C15—C16—H16120.0
C3—C2—Cl1119.63 (2)C17—C16—C15119.91 (3)
C3—C2—C1121.66 (3)C17—C16—H16120.0
C2—C3—H3120.2C16—C17—H17119.7
C2—C3—C4119.50 (3)C16—C17—C18120.60 (2)
C4—C3—H3120.2C18—C17—H17119.7
C3—C4—H4120.1C17—C18—H18120.0
C5—C4—C3119.73 (3)C19—C18—C17120.03 (3)
C5—C4—H4120.1C19—C18—H18120.0
C4—C5—Cl2119.42 (2)C14—C19—H19120.4
C4—C5—C6121.31 (3)C18—C19—C14119.20 (2)
C6—C5—Cl2119.27 (2)C18—C19—H19120.4
C1—C6—S2119.159 (18)C21—C20—P13118.03 (2)
C5—C6—S2122.02 (2)C25—C20—P13121.40 (2)
C5—C6—C1118.81 (2)C25—C20—C21120.48 (2)
S3ii—Ni2—S3180.0C20—C21—H21120.2
S3ii—Ni2—S4ii92.365 (3)C22—C21—C20119.66 (3)
S3—Ni2—S492.366 (3)C22—C21—H21120.2
S3ii—Ni2—S487.635 (3)C21—C22—H22120.1
S3—Ni2—S4ii87.634 (3)C21—C22—C23119.87 (3)
S4ii—Ni2—S4180.0C23—C22—H22120.1
C12—S3—Ni2104.862 (8)C22—C23—H23119.8
C7—S4—Ni2104.730 (9)C24—C23—C22120.47 (3)
C8—C7—S4122.051 (19)C24—C23—H23119.8
C8—C7—C12118.96 (2)C23—C24—H24119.9
C12—C7—S4118.980 (18)C23—C24—C25120.14 (3)
C7—C8—Cl4119.797 (19)C25—C24—H24119.9
C9—C8—Cl4118.95 (2)C20—C25—H25120.3
C9—C8—C7121.25 (2)C24—C25—C20119.37 (2)
C8—C9—H9120.1C24—C25—H25120.3
C8—C9—C10119.79 (2)C27—C26—P13119.811 (19)
C10—C9—H9120.1C27—C26—C31120.44 (2)
C9—C10—H10120.1C31—C26—P13119.731 (18)
C11—C10—C9119.73 (2)C26—C27—H27120.2
C11—C10—H10120.1C28—C27—C26119.65 (2)
C10—C11—Cl3118.940 (19)C28—C27—H27120.2
C10—C11—C12121.31 (2)C27—C28—H28120.0
C12—C11—Cl3119.74 (2)C27—C28—C29119.93 (2)
C7—C12—S3119.031 (18)C29—C28—H28120.0
C11—C12—S3122.124 (19)C28—C29—H29119.7
C11—C12—C7118.84 (2)C28—C29—C30120.53 (2)
C14—P13—C13109.157 (14)C30—C29—H29119.7
C14—P13—C26109.565 (12)C29—C30—H30120.0
C20—P13—C13109.920 (14)C31—C30—C29120.00 (2)
C20—P13—C14108.500 (12)C31—C30—H30120.0
C20—P13—C26111.293 (12)C26—C31—H31120.3
C26—P13—C13108.380 (13)C30—C31—C26119.40 (2)
P13—C13—H13A109.5C30—C31—H31120.3
Symmetry codes: (i) x+1, y+1, z+2; (ii) x, y+1, z+1.
 

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