Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229619006211/ky3175sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229619006211/ky3175Isup2.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S2053229619006211/ky3175sup3.pdf |
CCDC reference: 1911358
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT (Bruker, 2000); program(s) used to solve structure: SHELXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2017 (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).
[Ni(C9H9N)(C30H30ClN2P2)]PF6·0.7H2O | Z = 2 |
Mr = 863.42 | F(000) = 890 |
Triclinic, P1 | Dx = 1.477 Mg m−3 |
a = 9.7632 (5) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 10.8846 (5) Å | Cell parameters from 24485 reflections |
c = 18.5771 (9) Å | θ = 1.9–26.0° |
α = 99.687 (1)° | µ = 0.76 mm−1 |
β = 91.504 (1)° | T = 100 K |
γ = 93.472 (1)° | Prism, brown |
V = 1941.11 (16) Å3 | 0.38 × 0.3 × 0.25 mm |
Bruker APEXII CCD area detector diffractometer | 6603 reflections with I > 2σ(I) |
Radiation source: Fine focused sealed tube | Rint = 0.027 |
hemisphere scans | θmax = 26.0°, θmin = 1.9° |
Absorption correction: multi-scan (SADABS; Krause et al., 2015) | h = −9→12 |
Tmin = 0.761, Tmax = 0.827 | k = −13→13 |
24485 measured reflections | l = −22→22 |
7473 independent reflections |
Refinement on F2 | Primary atom site location: dual |
Least-squares matrix: full | Hydrogen site location: mixed |
R[F2 > 2σ(F2)] = 0.030 | H-atom parameters constrained |
wR(F2) = 0.075 | w = 1/[σ2(Fo2) + (0.0324P)2 + 1.1895P] where P = (Fo2 + 2Fc2)/3 |
S = 1.07 | (Δ/σ)max = 0.001 |
7473 reflections | Δρmax = 0.46 e Å−3 |
548 parameters | Δρmin = −0.30 e Å−3 |
6 restraints |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ni1 | 0.55256 (2) | 0.31871 (2) | 0.26588 (2) | 0.01216 (7) | |
Cl1 | 0.69379 (5) | 0.48010 (4) | 0.34566 (2) | 0.02068 (11) | |
P1 | 0.36300 (5) | 0.41089 (4) | 0.25893 (2) | 0.01180 (10) | |
P2 | 0.69958 (5) | 0.18756 (4) | 0.22150 (3) | 0.01532 (11) | |
P3 | 0.08955 (5) | −0.27772 (4) | 0.12213 (3) | 0.02086 (12) | |
F6 | 0.036 (2) | −0.3978 (15) | 0.0644 (9) | 0.025 (2) | 0.55 (5) |
F5 | 0.109 (3) | −0.188 (3) | 0.0628 (15) | 0.032 (3) | 0.55 (5) |
F3 | 0.088 (2) | −0.3692 (17) | 0.1820 (9) | 0.0241 (19) | 0.55 (5) |
F2 | 0.2452 (11) | −0.3114 (18) | 0.1056 (10) | 0.032 (2) | 0.55 (5) |
F4 | −0.0652 (11) | −0.2419 (18) | 0.1362 (12) | 0.044 (3) | 0.55 (5) |
N3 | 0.44606 (16) | 0.15472 (14) | 0.36875 (9) | 0.0159 (3) | |
N1 | 0.53457 (16) | 0.50139 (13) | 0.17225 (8) | 0.0150 (3) | |
F1 | 0.1476 (19) | −0.1573 (11) | 0.1788 (8) | 0.040 (2) | 0.55 (5) |
N2 | 0.71308 (16) | 0.37449 (14) | 0.14738 (8) | 0.0162 (3) | |
C32 | 0.38943 (18) | 0.06971 (16) | 0.41075 (10) | 0.0155 (4) | |
C1 | 0.26903 (19) | 0.47385 (15) | 0.33755 (10) | 0.0140 (4) | |
C38 | 0.35888 (19) | 0.11449 (17) | 0.48307 (11) | 0.0181 (4) | |
C12 | 0.20483 (19) | 0.36069 (17) | 0.12668 (10) | 0.0165 (4) | |
H12 | 0.235275 | 0.439581 | 0.118441 | 0.020* | |
C33 | 0.3661 (2) | −0.05508 (17) | 0.37706 (11) | 0.0190 (4) | |
C2 | 0.3351 (2) | 0.49687 (17) | 0.40612 (10) | 0.0181 (4) | |
H2 | 0.426093 | 0.478010 | 0.411243 | 0.022* | |
C7 | 0.24123 (18) | 0.32191 (16) | 0.19222 (10) | 0.0136 (4) | |
C18 | 0.80227 (19) | 0.28382 (18) | 0.16859 (11) | 0.0188 (4) | |
H18A | 0.880463 | 0.325815 | 0.197929 | 0.023* | |
H18B | 0.835727 | 0.232500 | 0.125648 | 0.023* | |
C31 | 0.48922 (18) | 0.22008 (16) | 0.33020 (10) | 0.0149 (4) | |
C6 | 0.1329 (2) | 0.50450 (18) | 0.32994 (11) | 0.0205 (4) | |
H6 | 0.088562 | 0.490372 | 0.284087 | 0.025* | |
C13 | 0.42924 (19) | 0.54658 (16) | 0.22191 (10) | 0.0150 (4) | |
H13A | 0.356744 | 0.580439 | 0.196048 | 0.018* | |
H13B | 0.467956 | 0.611237 | 0.260734 | 0.018* | |
C9 | 0.11236 (19) | 0.12481 (17) | 0.15070 (11) | 0.0209 (4) | |
H9 | 0.080947 | 0.045993 | 0.158656 | 0.025* | |
C17 | 0.60348 (18) | 0.40447 (16) | 0.18644 (10) | 0.0137 (4) | |
C8 | 0.19203 (19) | 0.20390 (17) | 0.20411 (11) | 0.0173 (4) | |
H8 | 0.212933 | 0.178289 | 0.248196 | 0.021* | |
C35 | 0.3081 (2) | −0.13671 (18) | 0.41933 (12) | 0.0233 (4) | |
H35 | 0.289979 | −0.220368 | 0.398939 | 0.028* | |
C11 | 0.12359 (19) | 0.28188 (18) | 0.07404 (10) | 0.0201 (4) | |
H11 | 0.098397 | 0.308506 | 0.030849 | 0.024* | |
C10 | 0.07972 (19) | 0.16365 (18) | 0.08544 (11) | 0.0222 (4) | |
H10 | 0.028066 | 0.109994 | 0.049102 | 0.027* | |
C37 | 0.3021 (2) | 0.02781 (19) | 0.52254 (11) | 0.0229 (4) | |
H37 | 0.280853 | 0.053574 | 0.571022 | 0.028* | |
C25 | 0.6284 (2) | 0.05732 (17) | 0.15465 (10) | 0.0179 (4) | |
C26 | 0.4871 (2) | 0.04360 (17) | 0.14133 (11) | 0.0193 (4) | |
H26 | 0.431048 | 0.098797 | 0.168329 | 0.023* | |
C30 | 0.7118 (2) | −0.02539 (18) | 0.11313 (12) | 0.0255 (5) | |
H30 | 0.806621 | −0.016810 | 0.121014 | 0.031* | |
C19 | 0.8240 (2) | 0.13232 (19) | 0.28081 (11) | 0.0224 (4) | |
C4 | 0.1308 (2) | 0.57660 (17) | 0.45901 (11) | 0.0232 (4) | |
H4 | 0.084152 | 0.610234 | 0.499969 | 0.028* | |
C3 | 0.2654 (2) | 0.54791 (17) | 0.46685 (11) | 0.0217 (4) | |
H3 | 0.309288 | 0.562788 | 0.512807 | 0.026* | |
C36 | 0.2767 (2) | −0.09613 (19) | 0.49107 (12) | 0.0257 (5) | |
H36 | 0.238198 | −0.152603 | 0.518431 | 0.031* | |
C14 | 0.5814 (2) | 0.58512 (18) | 0.12208 (11) | 0.0238 (4) | |
H14A | 0.641321 | 0.653220 | 0.148386 | 0.029* | |
H14B | 0.503114 | 0.620324 | 0.101877 | 0.029* | |
C39 | 0.3842 (2) | 0.25003 (18) | 0.51604 (12) | 0.0283 (5) | |
H39A | 0.476880 | 0.277572 | 0.507843 | 0.042* | |
H39B | 0.370229 | 0.260670 | 0.567623 | 0.042* | |
H39C | 0.321671 | 0.298462 | 0.493734 | 0.042* | |
C28 | 0.5118 (2) | −0.13257 (18) | 0.04791 (12) | 0.0276 (5) | |
H28 | 0.473117 | −0.196220 | 0.012127 | 0.033* | |
C5 | 0.0643 (2) | 0.55601 (19) | 0.39104 (12) | 0.0258 (5) | |
H5 | −0.026199 | 0.576635 | 0.386303 | 0.031* | |
C27 | 0.4288 (2) | −0.05118 (18) | 0.08840 (11) | 0.0241 (4) | |
H27 | 0.334121 | −0.059979 | 0.080142 | 0.029* | |
C20 | 0.9067 (2) | 0.2225 (2) | 0.32790 (11) | 0.0289 (5) | |
H20 | 0.895368 | 0.306770 | 0.328083 | 0.035* | |
C16 | 0.7709 (2) | 0.4468 (2) | 0.09361 (12) | 0.0258 (5) | |
H16A | 0.812815 | 0.391353 | 0.055220 | 0.031* | |
H16B | 0.841248 | 0.508151 | 0.117298 | 0.031* | |
C15 | 0.6580 (2) | 0.5119 (2) | 0.06104 (12) | 0.0278 (5) | |
H15A | 0.595132 | 0.450710 | 0.030908 | 0.033* | |
H15B | 0.697195 | 0.567956 | 0.030464 | 0.033* | |
C34 | 0.4018 (3) | −0.0976 (2) | 0.29920 (12) | 0.0329 (5) | |
H34A | 0.360008 | −0.046466 | 0.268601 | 0.049* | |
H34B | 0.368621 | −0.183124 | 0.283952 | 0.049* | |
H34C | 0.499716 | −0.090470 | 0.295207 | 0.049* | |
C29 | 0.6531 (2) | −0.11956 (19) | 0.06054 (13) | 0.0309 (5) | |
H29 | 0.708560 | −0.174920 | 0.033252 | 0.037* | |
C23 | 0.9387 (2) | −0.0265 (2) | 0.32980 (15) | 0.0406 (6) | |
H23 | 0.949579 | −0.110410 | 0.331006 | 0.049* | |
C21 | 1.0052 (2) | 0.1878 (3) | 0.37425 (12) | 0.0362 (6) | |
H21 | 1.060609 | 0.248325 | 0.404852 | 0.043* | |
C24 | 0.8388 (2) | 0.0065 (2) | 0.28204 (13) | 0.0310 (5) | |
H24 | 0.783558 | −0.054714 | 0.251798 | 0.037* | |
C22 | 1.0204 (2) | 0.0630 (3) | 0.37465 (13) | 0.0399 (6) | |
H22 | 1.086540 | 0.039324 | 0.405578 | 0.048* | |
F3A | 0.058 (2) | −0.359 (2) | 0.1853 (11) | 0.026 (2) | 0.45 (5) |
F6A | 0.060 (3) | −0.3932 (17) | 0.0566 (11) | 0.021 (2) | 0.45 (5) |
F5A | 0.099 (4) | −0.197 (3) | 0.0574 (18) | 0.036 (5) | 0.45 (5) |
F2A | 0.2487 (12) | −0.305 (2) | 0.1246 (13) | 0.036 (3) | 0.45 (5) |
F4A | −0.0717 (12) | −0.258 (2) | 0.1210 (13) | 0.034 (3) | 0.45 (5) |
F1A | 0.115 (3) | −0.1645 (14) | 0.1886 (10) | 0.047 (4) | 0.45 (5) |
O1 | 0.7722 (3) | 0.7080 (2) | 0.26718 (16) | 0.0506 (10) | 0.702 (6) |
H1A | 0.845247 | 0.690852 | 0.244737 | 0.076* | 0.702 (6) |
H1B | 0.756170 | 0.647324 | 0.289812 | 0.076* | 0.702 (6) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.01062 (12) | 0.01432 (12) | 0.01261 (13) | 0.00193 (9) | 0.00260 (9) | 0.00463 (9) |
Cl1 | 0.0178 (2) | 0.0266 (2) | 0.0157 (2) | −0.00350 (18) | −0.00200 (18) | 0.00054 (18) |
P1 | 0.0113 (2) | 0.0128 (2) | 0.0116 (2) | 0.00111 (17) | 0.00153 (18) | 0.00263 (17) |
P2 | 0.0119 (2) | 0.0184 (2) | 0.0172 (2) | 0.00412 (18) | 0.00352 (19) | 0.00604 (19) |
P3 | 0.0233 (3) | 0.0153 (2) | 0.0239 (3) | 0.0010 (2) | −0.0062 (2) | 0.0043 (2) |
F6 | 0.027 (5) | 0.026 (2) | 0.020 (3) | −0.015 (2) | 0.012 (3) | 0.002 (2) |
F5 | 0.033 (4) | 0.023 (3) | 0.039 (5) | −0.011 (4) | −0.019 (4) | 0.013 (3) |
F3 | 0.028 (5) | 0.025 (3) | 0.023 (2) | 0.011 (3) | 0.006 (3) | 0.011 (2) |
F2 | 0.020 (2) | 0.042 (2) | 0.038 (5) | 0.003 (2) | −0.003 (2) | 0.022 (4) |
F4 | 0.033 (3) | 0.045 (4) | 0.051 (8) | 0.021 (2) | 0.002 (3) | −0.004 (4) |
N3 | 0.0152 (8) | 0.0156 (7) | 0.0184 (8) | 0.0025 (6) | 0.0022 (7) | 0.0060 (7) |
N1 | 0.0163 (8) | 0.0154 (7) | 0.0147 (8) | 0.0009 (6) | 0.0040 (6) | 0.0060 (6) |
F1 | 0.062 (5) | 0.026 (3) | 0.030 (3) | −0.009 (2) | −0.018 (3) | 0.005 (2) |
N2 | 0.0135 (8) | 0.0202 (8) | 0.0166 (8) | 0.0017 (6) | 0.0063 (6) | 0.0072 (6) |
C32 | 0.0128 (9) | 0.0166 (9) | 0.0188 (10) | 0.0008 (7) | 0.0010 (7) | 0.0084 (7) |
C1 | 0.0158 (9) | 0.0114 (8) | 0.0146 (9) | −0.0005 (7) | 0.0034 (7) | 0.0015 (7) |
C38 | 0.0148 (10) | 0.0207 (9) | 0.0200 (10) | 0.0028 (7) | 0.0003 (8) | 0.0065 (8) |
C12 | 0.0138 (9) | 0.0185 (9) | 0.0175 (10) | 0.0018 (7) | 0.0037 (8) | 0.0030 (7) |
C33 | 0.0171 (10) | 0.0193 (9) | 0.0215 (10) | 0.0022 (7) | −0.0023 (8) | 0.0060 (8) |
C2 | 0.0199 (10) | 0.0176 (9) | 0.0173 (10) | 0.0030 (7) | 0.0006 (8) | 0.0037 (7) |
C7 | 0.0093 (9) | 0.0168 (8) | 0.0140 (9) | 0.0041 (7) | 0.0023 (7) | −0.0004 (7) |
C18 | 0.0125 (9) | 0.0228 (9) | 0.0224 (10) | 0.0033 (7) | 0.0058 (8) | 0.0064 (8) |
C31 | 0.0134 (9) | 0.0159 (9) | 0.0150 (9) | 0.0045 (7) | 0.0004 (7) | 0.0006 (7) |
C6 | 0.0162 (10) | 0.0229 (10) | 0.0209 (10) | 0.0008 (8) | 0.0006 (8) | −0.0005 (8) |
C13 | 0.0149 (9) | 0.0136 (8) | 0.0169 (9) | 0.0005 (7) | 0.0021 (8) | 0.0035 (7) |
C9 | 0.0122 (9) | 0.0152 (9) | 0.0341 (12) | 0.0012 (7) | 0.0037 (8) | −0.0002 (8) |
C17 | 0.0126 (9) | 0.0156 (8) | 0.0125 (9) | −0.0019 (7) | −0.0002 (7) | 0.0022 (7) |
C8 | 0.0134 (9) | 0.0180 (9) | 0.0215 (10) | 0.0034 (7) | 0.0019 (8) | 0.0055 (8) |
C35 | 0.0232 (11) | 0.0167 (9) | 0.0313 (12) | −0.0015 (8) | −0.0025 (9) | 0.0091 (8) |
C11 | 0.0141 (10) | 0.0309 (11) | 0.0138 (9) | 0.0041 (8) | 0.0002 (8) | −0.0008 (8) |
C10 | 0.0124 (10) | 0.0267 (10) | 0.0231 (11) | 0.0022 (8) | 0.0009 (8) | −0.0086 (8) |
C37 | 0.0228 (11) | 0.0299 (11) | 0.0188 (10) | 0.0042 (8) | 0.0051 (8) | 0.0104 (8) |
C25 | 0.0201 (10) | 0.0167 (9) | 0.0186 (10) | 0.0035 (7) | 0.0062 (8) | 0.0061 (7) |
C26 | 0.0203 (10) | 0.0198 (9) | 0.0187 (10) | 0.0033 (8) | 0.0050 (8) | 0.0047 (8) |
C30 | 0.0219 (11) | 0.0209 (10) | 0.0347 (12) | 0.0045 (8) | 0.0124 (9) | 0.0051 (9) |
C19 | 0.0143 (10) | 0.0355 (11) | 0.0215 (10) | 0.0107 (8) | 0.0084 (8) | 0.0124 (9) |
C4 | 0.0271 (11) | 0.0169 (9) | 0.0233 (11) | −0.0051 (8) | 0.0142 (9) | −0.0030 (8) |
C3 | 0.0309 (12) | 0.0190 (9) | 0.0154 (10) | 0.0005 (8) | 0.0037 (8) | 0.0038 (8) |
C36 | 0.0219 (11) | 0.0277 (11) | 0.0324 (12) | −0.0007 (8) | 0.0039 (9) | 0.0201 (9) |
C14 | 0.0272 (11) | 0.0230 (10) | 0.0256 (11) | 0.0034 (8) | 0.0093 (9) | 0.0149 (9) |
C39 | 0.0397 (13) | 0.0222 (10) | 0.0233 (11) | 0.0040 (9) | 0.0028 (10) | 0.0038 (9) |
C28 | 0.0413 (13) | 0.0168 (9) | 0.0234 (11) | −0.0044 (9) | 0.0053 (10) | 0.0014 (8) |
C5 | 0.0152 (10) | 0.0252 (10) | 0.0337 (12) | −0.0009 (8) | 0.0070 (9) | −0.0048 (9) |
C27 | 0.0249 (11) | 0.0240 (10) | 0.0248 (11) | −0.0005 (8) | 0.0017 (9) | 0.0086 (8) |
C20 | 0.0204 (11) | 0.0455 (13) | 0.0216 (11) | 0.0131 (10) | 0.0019 (9) | 0.0036 (10) |
C16 | 0.0229 (11) | 0.0324 (11) | 0.0261 (11) | 0.0040 (9) | 0.0136 (9) | 0.0137 (9) |
C15 | 0.0320 (12) | 0.0342 (11) | 0.0231 (11) | 0.0079 (9) | 0.0120 (9) | 0.0177 (9) |
C34 | 0.0499 (15) | 0.0228 (11) | 0.0248 (12) | 0.0007 (10) | 0.0058 (11) | 0.0009 (9) |
C29 | 0.0376 (13) | 0.0198 (10) | 0.0347 (13) | 0.0038 (9) | 0.0191 (11) | −0.0002 (9) |
C23 | 0.0297 (13) | 0.0500 (15) | 0.0540 (16) | 0.0168 (11) | 0.0141 (12) | 0.0360 (13) |
C21 | 0.0213 (12) | 0.0648 (17) | 0.0238 (12) | 0.0162 (11) | 0.0034 (9) | 0.0064 (11) |
C24 | 0.0205 (11) | 0.0388 (12) | 0.0407 (14) | 0.0079 (9) | 0.0068 (10) | 0.0234 (11) |
C22 | 0.0202 (12) | 0.0762 (19) | 0.0308 (13) | 0.0149 (12) | 0.0050 (10) | 0.0262 (13) |
F3A | 0.029 (7) | 0.025 (3) | 0.027 (3) | 0.014 (4) | 0.006 (4) | 0.007 (2) |
F6A | 0.024 (6) | 0.018 (3) | 0.018 (3) | −0.010 (3) | 0.013 (3) | 0.001 (2) |
F5A | 0.042 (8) | 0.030 (7) | 0.036 (5) | −0.016 (4) | −0.023 (4) | 0.023 (7) |
F2A | 0.019 (3) | 0.048 (4) | 0.047 (8) | −0.008 (2) | −0.017 (3) | 0.032 (6) |
F4A | 0.031 (3) | 0.039 (5) | 0.034 (6) | 0.014 (2) | 0.006 (3) | 0.006 (5) |
F1A | 0.088 (10) | 0.016 (3) | 0.033 (4) | −0.013 (4) | −0.012 (5) | −0.002 (3) |
O1 | 0.061 (2) | 0.0390 (16) | 0.054 (2) | −0.0134 (13) | −0.0005 (14) | 0.0197 (13) |
Ni1—Cl1 | 2.4305 (5) | C9—C10 | 1.385 (3) |
Ni1—P1 | 2.1690 (5) | C8—H8 | 0.9300 |
Ni1—P2 | 2.1660 (5) | C35—H35 | 0.9300 |
Ni1—C31 | 1.8311 (19) | C35—C36 | 1.380 (3) |
Ni1—C17 | 1.9344 (18) | C11—H11 | 0.9300 |
P1—C1 | 1.8039 (19) | C11—C10 | 1.383 (3) |
P1—C7 | 1.8074 (18) | C10—H10 | 0.9300 |
P1—C13 | 1.8226 (18) | C37—H37 | 0.9300 |
P2—C18 | 1.8276 (19) | C37—C36 | 1.382 (3) |
P2—C25 | 1.811 (2) | C25—C26 | 1.389 (3) |
P2—C19 | 1.814 (2) | C25—C30 | 1.399 (3) |
P3—F6 | 1.596 (9) | C26—H26 | 0.9300 |
P3—F5 | 1.600 (9) | C26—C27 | 1.383 (3) |
P3—F3 | 1.613 (8) | C30—H30 | 0.9300 |
P3—F2 | 1.610 (8) | C30—C29 | 1.377 (3) |
P3—F4 | 1.600 (9) | C19—C20 | 1.400 (3) |
P3—F1 | 1.601 (8) | C19—C24 | 1.390 (3) |
P3—F3A | 1.606 (11) | C4—H4 | 0.9300 |
P3—F6A | 1.601 (11) | C4—C3 | 1.378 (3) |
P3—F5A | 1.609 (11) | C4—C5 | 1.382 (3) |
P3—F2A | 1.600 (11) | C3—H3 | 0.9300 |
P3—F4A | 1.602 (11) | C36—H36 | 0.9300 |
P3—F1A | 1.593 (10) | C14—H14A | 0.9700 |
N3—C32 | 1.405 (2) | C14—H14B | 0.9700 |
N1—C13 | 1.452 (2) | C14—C15 | 1.514 (3) |
N1—C17 | 1.344 (2) | C39—H39A | 0.9600 |
N1—C14 | 1.472 (2) | C39—H39B | 0.9600 |
N2—C17 | 1.335 (2) | C39—H39C | 0.9600 |
N2—C18 | 1.451 (2) | C28—H28 | 0.9300 |
N2—C16 | 1.475 (2) | C28—C27 | 1.379 (3) |
N3—C31 | 1.161 (2) | C28—C29 | 1.387 (3) |
C32—C38 | 1.396 (3) | C5—H5 | 0.9300 |
C32—C33 | 1.399 (3) | C27—H27 | 0.9300 |
C1—C2 | 1.390 (3) | C20—H20 | 0.9300 |
C1—C6 | 1.399 (3) | C20—C21 | 1.385 (3) |
C38—C37 | 1.388 (3) | C16—H16A | 0.9700 |
C38—C39 | 1.502 (3) | C16—H16B | 0.9700 |
C12—H12 | 0.9300 | C16—C15 | 1.513 (3) |
C12—C7 | 1.398 (3) | C15—H15A | 0.9700 |
C12—C11 | 1.384 (3) | C15—H15B | 0.9700 |
C33—C35 | 1.387 (3) | C34—H34A | 0.9600 |
C33—C34 | 1.500 (3) | C34—H34B | 0.9600 |
C2—H2 | 0.9300 | C34—H34C | 0.9600 |
C2—C3 | 1.386 (3) | C29—H29 | 0.9300 |
C7—C8 | 1.399 (3) | C23—H23 | 0.9300 |
C18—H18A | 0.9700 | C23—C24 | 1.404 (3) |
C18—H18B | 0.9700 | C23—C22 | 1.370 (4) |
C6—H6 | 0.9300 | C21—H21 | 0.9300 |
C6—C5 | 1.387 (3) | C21—C22 | 1.376 (4) |
C13—H13A | 0.9700 | C24—H24 | 0.9300 |
C13—H13B | 0.9700 | C22—H22 | 0.9300 |
C9—H9 | 0.9300 | O1—H1A | 0.8504 |
C9—C8 | 1.386 (3) | O1—H1B | 0.8497 |
P1—Ni1—Cl1 | 100.968 (19) | C10—C9—C8 | 119.72 (18) |
P2—Ni1—Cl1 | 103.29 (2) | N1—C17—Ni1 | 120.68 (13) |
P2—Ni1—P1 | 152.21 (2) | N2—C17—Ni1 | 121.04 (13) |
C31—Ni1—Cl1 | 101.89 (6) | N2—C17—N1 | 118.13 (16) |
C31—Ni1—P1 | 94.89 (6) | C7—C8—H8 | 119.7 |
C31—Ni1—P2 | 93.19 (6) | C9—C8—C7 | 120.51 (18) |
C31—Ni1—C17 | 171.10 (8) | C9—C8—H8 | 119.7 |
C17—Ni1—Cl1 | 87.02 (5) | C33—C35—H35 | 119.4 |
C17—Ni1—P1 | 83.42 (5) | C36—C35—C33 | 121.26 (18) |
C17—Ni1—P2 | 84.51 (5) | C36—C35—H35 | 119.4 |
C1—P1—Ni1 | 123.61 (6) | C12—C11—H11 | 119.9 |
C1—P1—C7 | 107.69 (8) | C10—C11—C12 | 120.25 (18) |
C1—P1—C13 | 105.08 (8) | C10—C11—H11 | 119.9 |
C7—P1—Ni1 | 112.12 (6) | C9—C10—H10 | 119.8 |
C7—P1—C13 | 107.81 (8) | C11—C10—C9 | 120.33 (18) |
C13—P1—Ni1 | 98.98 (6) | C11—C10—H10 | 119.8 |
C18—P2—Ni1 | 100.44 (6) | C38—C37—H37 | 119.4 |
C25—P2—Ni1 | 114.87 (6) | C36—C37—C38 | 121.15 (19) |
C25—P2—C18 | 104.57 (9) | C36—C37—H37 | 119.4 |
C25—P2—C19 | 109.27 (9) | C26—C25—P2 | 118.84 (14) |
C19—P2—Ni1 | 120.87 (7) | C26—C25—C30 | 119.10 (18) |
C19—P2—C18 | 104.45 (9) | C30—C25—P2 | 121.95 (16) |
F6—P3—F5 | 95.0 (17) | C25—C26—H26 | 119.6 |
F6—P3—F3 | 86.3 (11) | C27—C26—C25 | 120.79 (18) |
F6—P3—F2 | 89.4 (9) | C27—C26—H26 | 119.6 |
F6—P3—F4 | 90.5 (9) | C25—C30—H30 | 120.1 |
F6—P3—F1 | 178.2 (8) | C29—C30—C25 | 119.8 (2) |
F5—P3—F3 | 173.9 (14) | C29—C30—H30 | 120.1 |
F5—P3—F2 | 85.4 (12) | C20—C19—P2 | 117.36 (15) |
F5—P3—F1 | 84.2 (16) | C24—C19—P2 | 123.23 (17) |
F2—P3—F3 | 88.7 (7) | C24—C19—C20 | 119.40 (19) |
F4—P3—F5 | 92.7 (12) | C3—C4—H4 | 119.6 |
F4—P3—F3 | 93.2 (8) | C3—C4—C5 | 120.83 (19) |
F4—P3—F2 | 178.1 (8) | C5—C4—H4 | 119.6 |
F4—P3—F1 | 91.2 (9) | C2—C3—H3 | 120.1 |
F1—P3—F3 | 94.3 (10) | C4—C3—C2 | 119.87 (19) |
F1—P3—F2 | 89.0 (8) | C4—C3—H3 | 120.1 |
F3A—P3—F5A | 172.4 (18) | C35—C36—C37 | 120.48 (18) |
F6A—P3—F3A | 94.6 (13) | C35—C36—H36 | 119.8 |
F6A—P3—F5A | 84 (2) | C37—C36—H36 | 119.8 |
F6A—P3—F4A | 88.4 (11) | N1—C14—H14A | 109.8 |
F2A—P3—F3A | 91.5 (9) | N1—C14—H14B | 109.8 |
F2A—P3—F6A | 90.3 (11) | N1—C14—C15 | 109.24 (15) |
F2A—P3—F5A | 96.0 (17) | H14A—C14—H14B | 108.3 |
F2A—P3—F4A | 176.9 (11) | C15—C14—H14A | 109.8 |
F4A—P3—F3A | 85.8 (10) | C15—C14—H14B | 109.8 |
F4A—P3—F5A | 86.7 (16) | C38—C39—H39A | 109.5 |
F1A—P3—F3A | 84.0 (13) | C38—C39—H39B | 109.5 |
F1A—P3—F6A | 178.3 (10) | C38—C39—H39C | 109.5 |
F1A—P3—F5A | 97.3 (19) | H39A—C39—H39B | 109.5 |
F1A—P3—F2A | 90.7 (10) | H39A—C39—H39C | 109.5 |
F1A—P3—F4A | 90.5 (11) | H39B—C39—H39C | 109.5 |
C31—N3—C32 | 175.71 (18) | C27—C28—H28 | 120.0 |
C13—N1—C14 | 116.07 (14) | C27—C28—C29 | 120.0 (2) |
C17—N1—C13 | 118.15 (15) | C29—C28—H28 | 120.0 |
C17—N1—C14 | 123.79 (16) | C6—C5—H5 | 120.1 |
C18—N2—C16 | 114.51 (15) | C4—C5—C6 | 119.78 (19) |
C17—N2—C18 | 119.58 (15) | C4—C5—H5 | 120.1 |
C17—N2—C16 | 124.39 (15) | C26—C27—H27 | 120.1 |
C38—C32—N3 | 118.38 (16) | C28—C27—C26 | 119.7 (2) |
C38—C32—C33 | 123.96 (17) | C28—C27—H27 | 120.1 |
C33—C32—N3 | 117.66 (17) | C19—C20—H20 | 119.6 |
C2—C1—P1 | 119.25 (14) | C21—C20—C19 | 120.8 (2) |
C2—C1—C6 | 119.76 (17) | C21—C20—H20 | 119.6 |
C6—C1—P1 | 120.93 (14) | N2—C16—H16A | 109.8 |
C32—C38—C39 | 121.63 (17) | N2—C16—H16B | 109.8 |
C37—C38—C32 | 116.62 (17) | N2—C16—C15 | 109.58 (16) |
C37—C38—C39 | 121.75 (18) | H16A—C16—H16B | 108.2 |
C7—C12—H12 | 119.9 | C15—C16—H16A | 109.8 |
C11—C12—H12 | 119.9 | C15—C16—H16B | 109.8 |
C11—C12—C7 | 120.13 (17) | C14—C15—H15A | 109.8 |
C32—C33—C34 | 121.45 (17) | C14—C15—H15B | 109.8 |
C35—C33—C32 | 116.53 (18) | C16—C15—C14 | 109.25 (17) |
C35—C33—C34 | 122.02 (18) | C16—C15—H15A | 109.8 |
C1—C2—H2 | 120.0 | C16—C15—H15B | 109.8 |
C3—C2—C1 | 120.01 (18) | H15A—C15—H15B | 108.3 |
C3—C2—H2 | 120.0 | C33—C34—H34A | 109.5 |
C12—C7—P1 | 122.88 (14) | C33—C34—H34B | 109.5 |
C12—C7—C8 | 119.00 (17) | C33—C34—H34C | 109.5 |
C8—C7—P1 | 117.83 (14) | H34A—C34—H34B | 109.5 |
P2—C18—H18A | 110.4 | H34A—C34—H34C | 109.5 |
P2—C18—H18B | 110.4 | H34B—C34—H34C | 109.5 |
N2—C18—P2 | 106.75 (12) | C30—C29—C28 | 120.59 (19) |
N2—C18—H18A | 110.4 | C30—C29—H29 | 119.7 |
N2—C18—H18B | 110.4 | C28—C29—H29 | 119.7 |
H18A—C18—H18B | 108.6 | C24—C23—H23 | 119.5 |
N3—C31—Ni1 | 177.33 (17) | C22—C23—H23 | 119.5 |
C1—C6—H6 | 120.1 | C22—C23—C24 | 121.0 (2) |
C5—C6—C1 | 119.74 (18) | C20—C21—H21 | 120.3 |
C5—C6—H6 | 120.1 | C22—C21—C20 | 119.5 (2) |
P1—C13—H13A | 110.6 | C22—C21—H21 | 120.3 |
P1—C13—H13B | 110.6 | C19—C24—C23 | 118.8 (2) |
N1—C13—P1 | 105.48 (11) | C19—C24—H24 | 120.6 |
N1—C13—H13A | 110.6 | C23—C24—H24 | 120.6 |
N1—C13—H13B | 110.6 | C23—C22—C21 | 120.5 (2) |
H13A—C13—H13B | 108.8 | C23—C22—H22 | 119.8 |
C8—C9—H9 | 120.1 | C21—C22—H22 | 119.8 |
C10—C9—H9 | 120.1 | H1A—O1—H1B | 104.4 |
Ni1—P1—C1—C2 | 18.36 (17) | C18—N2—C17—Ni1 | −5.4 (2) |
Ni1—P1—C1—C6 | −164.32 (12) | C18—N2—C17—N1 | 170.37 (16) |
Ni1—P1—C7—C12 | −110.89 (14) | C18—N2—C16—C15 | 165.17 (17) |
Ni1—P1—C7—C8 | 62.89 (15) | C6—C1—C2—C3 | 1.2 (3) |
Ni1—P1—C13—N1 | 36.09 (12) | C13—P1—C1—C2 | −93.55 (15) |
Ni1—P2—C18—N2 | −27.67 (13) | C13—P1—C1—C6 | 83.77 (16) |
Ni1—P2—C25—C26 | −5.68 (17) | C13—P1—C7—C12 | −2.98 (18) |
Ni1—P2—C25—C30 | 170.53 (14) | C13—P1—C7—C8 | 170.80 (14) |
Ni1—P2—C19—C20 | −53.86 (18) | C13—N1—C17—Ni1 | 5.3 (2) |
Ni1—P2—C19—C24 | 125.23 (16) | C13—N1—C17—N2 | −170.45 (16) |
P1—C1—C2—C3 | 178.51 (14) | C13—N1—C14—C15 | −163.90 (17) |
P1—C1—C6—C5 | −178.20 (15) | C17—N1—C13—P1 | −29.47 (19) |
P1—C7—C8—C9 | −171.79 (14) | C17—N1—C14—C15 | 32.5 (3) |
P2—C25—C26—C27 | 177.05 (14) | C17—N2—C18—P2 | 23.4 (2) |
P2—C25—C30—C29 | −176.95 (16) | C17—N2—C16—C15 | −29.0 (3) |
P2—C19—C20—C21 | −179.24 (17) | C8—C9—C10—C11 | −1.5 (3) |
P2—C19—C24—C23 | 179.73 (17) | C11—C12—C7—P1 | 172.42 (14) |
N3—C32—C38—C37 | 179.53 (16) | C11—C12—C7—C8 | −1.3 (3) |
N3—C32—C38—C39 | 0.4 (3) | C10—C9—C8—C7 | −0.9 (3) |
N3—C32—C33—C35 | −178.99 (16) | C25—P2—C18—N2 | 91.66 (14) |
N3—C32—C33—C34 | 0.8 (3) | C25—P2—C19—C20 | 169.40 (15) |
N1—C14—C15—C16 | −53.8 (2) | C25—P2—C19—C24 | −11.5 (2) |
N2—C16—C15—C14 | 52.2 (2) | C25—C26—C27—C28 | −0.5 (3) |
C32—C38—C37—C36 | −0.5 (3) | C25—C30—C29—C28 | 0.5 (3) |
C32—C33—C35—C36 | −0.6 (3) | C26—C25—C30—C29 | −0.7 (3) |
C1—P1—C7—C12 | 109.92 (16) | C30—C25—C26—C27 | 0.7 (3) |
C1—P1—C7—C8 | −76.30 (15) | C19—P2—C18—N2 | −153.56 (13) |
C1—P1—C13—N1 | 164.62 (12) | C19—P2—C25—C26 | 133.90 (15) |
C1—C2—C3—C4 | −0.5 (3) | C19—P2—C25—C30 | −49.89 (19) |
C1—C6—C5—C4 | −0.1 (3) | C19—C20—C21—C22 | −0.9 (3) |
C38—C32—C33—C35 | 0.5 (3) | C3—C4—C5—C6 | 0.8 (3) |
C38—C32—C33—C34 | −179.68 (19) | C14—N1—C13—P1 | 165.93 (13) |
C38—C37—C36—C35 | 0.3 (3) | C14—N1—C17—Ni1 | 168.61 (14) |
C12—C7—C8—C9 | 2.2 (3) | C14—N1—C17—N2 | −7.1 (3) |
C12—C11—C10—C9 | 2.4 (3) | C39—C38—C37—C36 | 178.63 (19) |
C33—C32—C38—C37 | 0.0 (3) | C5—C4—C3—C2 | −0.5 (3) |
C33—C32—C38—C39 | −179.05 (18) | C27—C28—C29—C30 | −0.3 (3) |
C33—C35—C36—C37 | 0.3 (3) | C20—C19—C24—C23 | −1.2 (3) |
C2—C1—C6—C5 | −0.9 (3) | C20—C21—C22—C23 | −0.2 (4) |
C7—P1—C1—C2 | 151.72 (14) | C16—N2—C18—P2 | −170.03 (14) |
C7—P1—C1—C6 | −30.96 (17) | C16—N2—C17—Ni1 | −170.47 (14) |
C7—P1—C13—N1 | −80.73 (13) | C16—N2—C17—N1 | 5.2 (3) |
C7—C12—C11—C10 | −1.0 (3) | C34—C33—C35—C36 | 179.6 (2) |
C18—P2—C25—C26 | −114.76 (15) | C29—C28—C27—C26 | 0.3 (3) |
C18—P2—C25—C30 | 61.46 (18) | C24—C19—C20—C21 | 1.6 (3) |
C18—P2—C19—C20 | 57.98 (18) | C24—C23—C22—C21 | 0.6 (4) |
C18—P2—C19—C24 | −122.93 (18) | C22—C23—C24—C19 | 0.1 (3) |
D—H···A | D—H | H···A | D···A | D—H···A |
C9—H9···F1 | 0.93 | 2.43 | 3.237 (15) | 145 |
C9—H9···F1A | 0.93 | 2.49 | 3.342 (19) | 153 |
C14—H14A···O1 | 0.97 | 2.48 | 3.278 (4) | 139 |
C20—H20···Cl1 | 0.93 | 2.80 | 3.567 (2) | 141 |
O1—H1B···Cl1 | 0.85 | 2.30 | 3.148 (3) | 175 |