Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229615001680/fg3327sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S2053229615001680/fg3327Isup2.hkl |
CCDC reference: 1045544
Crystal data, data collection and structure refinement details are summarized in Table 1. Two of the phenoxy rings on P2 and one on P1 were all modelled as being disordered over two sets of sites. Occupancy factors were set at 0.5 after trial refinement and intramolecular contact considerations. Geometries of the disordered components were restrained to ideal values with the atoms refined with isotropic displacement parameters after anisotropic refinement resulted in unacceptable ellipsoids even with reasonable restraints. There was no indication that the disorder resulted from a 2-fold rotation of the o-tolyl groups about the C—O bonds.
Data collection: CrysAlis PRO (Agilent, 2013); cell refinement: CrysAlis PRO (Agilent, 2013); data reduction: CrysAlis PRO (Agilent, 2013); program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 2012).
[Ni(C21H21O3P)3] | F(000) = 4688 |
Mr = 1115.75 | Dx = 1.323 Mg m−3 |
Monoclinic, C2/c | Cu Kα radiation, λ = 1.54178 Å |
Hall symbol: -C 2yc | Cell parameters from 15074 reflections |
a = 21.5898 (9) Å | θ = 4.1–67.1° |
b = 12.3292 (3) Å | µ = 1.77 mm−1 |
c = 43.403 (2) Å | T = 100 K |
β = 104.129 (5)° | Needle, orange |
V = 11203.8 (7) Å3 | 0.28 × 0.11 × 0.07 mm |
Z = 8 |
Oxford Gemini diffractometer | 9993 independent reflections |
Radiation source: sealed X-ray tube | 8185 reflections with I > 2σ(I) |
Mirror monochromator | Rint = 0.043 |
Detector resolution: 10.4738 pixels mm-1 | θmax = 67.4°, θmin = 4.2° |
ω scans | h = −25→25 |
Absorption correction: analytical (CrysAlis PRO; Agilent, 2013) | k = −14→9 |
Tmin = 0.726, Tmax = 0.896 | l = −51→51 |
56232 measured reflections |
Refinement on F2 | 82 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.099 | H-atom parameters constrained |
wR(F2) = 0.259 | w = 1/[σ2(Fo2) + (0.1046P)2 + 70.9791P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.003 |
9993 reflections | Δρmax = 1.26 e Å−3 |
682 parameters | Δρmin = −1.41 e Å−3 |
[Ni(C21H21O3P)3] | V = 11203.8 (7) Å3 |
Mr = 1115.75 | Z = 8 |
Monoclinic, C2/c | Cu Kα radiation |
a = 21.5898 (9) Å | µ = 1.77 mm−1 |
b = 12.3292 (3) Å | T = 100 K |
c = 43.403 (2) Å | 0.28 × 0.11 × 0.07 mm |
β = 104.129 (5)° |
Oxford Gemini diffractometer | 9993 independent reflections |
Absorption correction: analytical (CrysAlis PRO; Agilent, 2013) | 8185 reflections with I > 2σ(I) |
Tmin = 0.726, Tmax = 0.896 | Rint = 0.043 |
56232 measured reflections |
R[F2 > 2σ(F2)] = 0.099 | 82 restraints |
wR(F2) = 0.259 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.1046P)2 + 70.9791P] where P = (Fo2 + 2Fc2)/3 |
9993 reflections | Δρmax = 1.26 e Å−3 |
682 parameters | Δρmin = −1.41 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Ni1 | 0.16191 (5) | 0.01350 (7) | 0.13447 (2) | 0.0662 (3) | |
P1 | 0.12143 (6) | 0.07529 (12) | 0.08885 (3) | 0.0554 (4) | |
O11 | 0.1535 (4) | 0.0437 (7) | 0.06232 (18) | 0.0509 (19)* | 0.5 |
C111 | 0.1564 (5) | −0.0534 (10) | 0.0461 (2) | 0.051 (2)* | 0.5 |
C112 | 0.1878 (7) | −0.0500 (11) | 0.0224 (3) | 0.087 (4)* | 0.5 |
C113 | 0.1882 (9) | −0.1420 (14) | 0.0031 (4) | 0.106 (6)* | 0.5 |
H113 | 0.205 | −0.1397 | −0.0152 | 0.127* | 0.5 |
C114 | 0.1626 (8) | −0.2364 (12) | 0.0126 (4) | 0.107 (5)* | 0.5 |
H114 | 0.1676 | −0.3019 | 0.0019 | 0.128* | 0.5 |
C115 | 0.1305 (7) | −0.2413 (10) | 0.0363 (3) | 0.088 (4)* | 0.5 |
H115 | 0.112 | −0.3073 | 0.0411 | 0.106* | 0.5 |
C116 | 0.1260 (5) | −0.1466 (8) | 0.0532 (2) | 0.057 (3)* | 0.5 |
H116 | 0.1027 | −0.1457 | 0.0692 | 0.068* | 0.5 |
C117 | 0.2158 (8) | 0.0607 (14) | 0.0139 (4) | 0.084 (4)* | 0.5 |
H11A | 0.2501 | 0.0843 | 0.0319 | 0.126* | 0.5 |
H11B | 0.1819 | 0.1155 | 0.0095 | 0.126* | 0.5 |
H11C | 0.2328 | 0.0511 | −0.0049 | 0.126* | 0.5 |
O41 | 0.1572 (3) | 0.0836 (7) | 0.05713 (18) | 0.0484 (18)* | 0.5 |
C141 | 0.1642 (5) | −0.0077 (8) | 0.0398 (2) | 0.049 (2)* | 0.5 |
C142 | 0.1933 (6) | 0.0071 (9) | 0.0154 (3) | 0.060 (3)* | 0.5 |
C143 | 0.1994 (6) | −0.0788 (10) | −0.0042 (3) | 0.077 (3)* | 0.5 |
H143 | 0.2155 | −0.068 | −0.0225 | 0.093* | 0.5 |
C144 | 0.1807 (6) | −0.1844 (10) | 0.0039 (3) | 0.064 (3)* | 0.5 |
H144 | 0.1894 | −0.2457 | −0.0076 | 0.077* | 0.5 |
C145 | 0.1514 (6) | −0.1982 (9) | 0.0273 (3) | 0.074 (3)* | 0.5 |
H145 | 0.1342 | −0.2669 | 0.0306 | 0.089* | 0.5 |
C146 | 0.1462 (5) | −0.1107 (9) | 0.0468 (2) | 0.048 (2)* | 0.5 |
H146 | 0.1301 | −0.1219 | 0.065 | 0.058* | 0.5 |
C147 | 0.2130 (7) | 0.1270 (12) | 0.0085 (3) | 0.074 (3)* | 0.5 |
H14A | 0.2495 | 0.1502 | 0.0255 | 0.112* | 0.5 |
H14B | 0.1769 | 0.176 | 0.0078 | 0.112* | 0.5 |
H14C | 0.2248 | 0.129 | −0.0119 | 0.112* | 0.5 |
O12 | 0.05100 (16) | 0.0424 (3) | 0.06782 (8) | 0.0545 (8) | |
C121 | −0.0027 (3) | 0.0245 (5) | 0.07937 (13) | 0.0577 (13) | |
C122 | −0.0489 (3) | −0.0423 (6) | 0.06046 (15) | 0.0792 (19) | |
C123 | −0.1043 (4) | −0.0602 (9) | 0.0711 (2) | 0.123 (4) | |
H123 | −0.137 | −0.1049 | 0.0589 | 0.147* | |
C124 | −0.1126 (4) | −0.0151 (9) | 0.0987 (2) | 0.121 (4) | |
H124 | −0.1508 | −0.0287 | 0.1053 | 0.145* | |
C125 | −0.0658 (4) | 0.0495 (8) | 0.11691 (17) | 0.096 (2) | |
H125 | −0.0712 | 0.0794 | 0.1363 | 0.116* | |
C126 | −0.0104 (3) | 0.0712 (5) | 0.10677 (13) | 0.0658 (14) | |
H126 | 0.0216 | 0.1179 | 0.1188 | 0.079* | |
C127 | −0.0392 (4) | −0.0932 (8) | 0.03009 (18) | 0.104 (3) | |
H12A | −0.0709 | −0.1505 | 0.0231 | 0.156* | |
H12B | 0.0038 | −0.1243 | 0.0341 | 0.156* | |
H12C | −0.0442 | −0.0376 | 0.0135 | 0.156* | |
O13 | 0.11931 (18) | 0.2075 (3) | 0.08807 (8) | 0.0590 (9) | |
C131 | 0.0991 (3) | 0.2709 (5) | 0.06014 (14) | 0.0659 (15) | |
C132 | 0.1439 (4) | 0.3287 (7) | 0.04999 (17) | 0.092 (2) | |
C133 | 0.1223 (5) | 0.3921 (8) | 0.0223 (2) | 0.109 (3) | |
H133 | 0.1524 | 0.432 | 0.0142 | 0.131* | |
C134 | 0.0592 (4) | 0.3971 (7) | 0.00709 (18) | 0.093 (2) | |
H134 | 0.0459 | 0.4399 | −0.0116 | 0.112* | |
C135 | 0.0153 (4) | 0.3415 (6) | 0.01838 (16) | 0.0831 (19) | |
H135 | −0.0287 | 0.3466 | 0.0079 | 0.1* | |
C136 | 0.0345 (3) | 0.2771 (5) | 0.04520 (14) | 0.0673 (15) | |
H136 | 0.004 | 0.2378 | 0.0532 | 0.081* | |
C137 | 0.2125 (4) | 0.3238 (10) | 0.0674 (2) | 0.133 (4) | |
H13A | 0.2159 | 0.3237 | 0.0903 | 0.2* | |
H13B | 0.235 | 0.3872 | 0.0618 | 0.2* | |
H13C | 0.2318 | 0.2575 | 0.0615 | 0.2* | |
P2 | 0.2204 (3) | −0.1216 (6) | 0.14246 (17) | 0.0443 (11) | 0.5 |
P2' | 0.2379 (3) | −0.1055 (6) | 0.13774 (18) | 0.0539 (14) | 0.5 |
O21 | 0.27639 (15) | −0.1313 (3) | 0.17414 (8) | 0.0475 (7) | |
C211 | 0.3215 (2) | −0.2155 (4) | 0.18260 (11) | 0.0489 (11) | |
C212 | 0.3076 (3) | −0.3061 (4) | 0.19741 (14) | 0.0616 (14) | |
C213 | 0.3563 (4) | −0.3821 (5) | 0.20770 (15) | 0.080 (2) | |
H213 | 0.3472 | −0.4466 | 0.2177 | 0.096* | |
C214 | 0.4154 (4) | −0.3670 (7) | 0.20392 (17) | 0.092 (2) | |
H214 | 0.4478 | −0.4196 | 0.2113 | 0.11* | |
C215 | 0.4285 (3) | −0.2741 (8) | 0.1892 (2) | 0.102 (3) | |
H215 | 0.4704 | −0.2623 | 0.1865 | 0.122* | |
C216 | 0.3818 (3) | −0.1985 (5) | 0.17827 (16) | 0.0709 (16) | |
H216 | 0.3909 | −0.1349 | 0.1678 | 0.085* | |
C217 | 0.2442 (4) | −0.3264 (6) | 0.2043 (2) | 0.106 (3) | |
H21A | 0.2217 | −0.2574 | 0.2042 | 0.16* | |
H21B | 0.2504 | −0.3609 | 0.2251 | 0.16* | |
H21C | 0.2189 | −0.3743 | 0.1879 | 0.16* | |
O22 | 0.1922 (3) | −0.2400 (5) | 0.14174 (14) | 0.0385 (12)* | 0.5 |
C221 | 0.1277 (4) | −0.2482 (8) | 0.1297 (3) | 0.058 (3)* | 0.5 |
C222 | 0.1058 (5) | −0.3344 (9) | 0.1094 (3) | 0.066 (3)* | 0.5 |
C223 | 0.0385 (6) | −0.3432 (12) | 0.1008 (4) | 0.092 (5)* | 0.5 |
H223 | 0.0206 | −0.4059 | 0.0893 | 0.11* | 0.5 |
C224 | −0.0016 (7) | −0.2705 (14) | 0.1075 (5) | 0.118 (6)* | 0.5 |
H224 | −0.0462 | −0.2767 | 0.0986 | 0.141* | 0.5 |
C225 | 0.0227 (6) | −0.1847 (11) | 0.1280 (3) | 0.090 (4)* | 0.5 |
H225 | −0.0053 | −0.1345 | 0.1342 | 0.109* | 0.5 |
C226 | 0.0863 (5) | −0.1744 (9) | 0.1387 (3) | 0.068 (3)* | 0.5 |
H226 | 0.1033 | −0.1163 | 0.1526 | 0.081* | 0.5 |
C227 | 0.1518 (8) | −0.4181 (15) | 0.1029 (4) | 0.096 (4)* | 0.5 |
H22A | 0.1616 | −0.4704 | 0.1204 | 0.144* | 0.5 |
H22B | 0.1912 | −0.3823 | 0.101 | 0.144* | 0.5 |
H22C | 0.1324 | −0.456 | 0.083 | 0.144* | 0.5 |
O24 | 0.2143 (6) | −0.2238 (11) | 0.1255 (3) | 0.125 (4)* | 0.5 |
C241 | 0.1500 (7) | −0.2572 (14) | 0.1163 (4) | 0.111 (5)* | 0.5 |
C242 | 0.1501 (7) | −0.3444 (17) | 0.0954 (5) | 0.118 (6)* | 0.5 |
C243 | 0.0904 (9) | −0.3860 (18) | 0.0793 (5) | 0.156 (9)* | 0.5 |
H243 | 0.0872 | −0.4421 | 0.064 | 0.187* | 0.5 |
C244 | 0.0398 (7) | −0.3458 (14) | 0.0858 (4) | 0.100 (5)* | 0.5 |
H244 | 0.0002 | −0.3747 | 0.0742 | 0.12* | 0.5 |
C245 | 0.0364 (10) | −0.264 (3) | 0.1081 (8) | 0.227 (16)* | 0.5 |
H245 | −0.003 | −0.2416 | 0.112 | 0.273* | 0.5 |
C246 | 0.0955 (11) | −0.219 (2) | 0.1241 (6) | 0.180 (12)* | 0.5 |
H246 | 0.0978 | −0.1645 | 0.1398 | 0.216* | 0.5 |
C247 | 0.1950 (12) | −0.394 (2) | 0.0864 (6) | 0.154 (9)* | 0.5 |
H24A | 0.1763 | −0.4443 | 0.0691 | 0.232* | 0.5 |
H24B | 0.2211 | −0.4351 | 0.1043 | 0.232* | 0.5 |
H24C | 0.2219 | −0.3413 | 0.0789 | 0.232* | 0.5 |
O23 | 0.2619 (3) | −0.1528 (6) | 0.11591 (15) | 0.0488 (15)* | 0.5 |
C231 | 0.3002 (7) | −0.0896 (11) | 0.1033 (4) | 0.080 (4)* | 0.5 |
C232 | 0.3354 (9) | −0.1481 (13) | 0.0852 (5) | 0.113 (6)* | 0.5 |
C233 | 0.3770 (10) | −0.0839 (16) | 0.0731 (5) | 0.144 (8)* | 0.5 |
H233 | 0.4045 | −0.1185 | 0.0621 | 0.173* | 0.5 |
C234 | 0.3803 (11) | 0.0244 (16) | 0.0763 (6) | 0.146 (9)* | 0.5 |
H234 | 0.4057 | 0.0644 | 0.0653 | 0.176* | 0.5 |
C235 | 0.3467 (10) | 0.0811 (13) | 0.0958 (5) | 0.128 (7)* | 0.5 |
H235 | 0.3506 | 0.1572 | 0.0991 | 0.153* | 0.5 |
C236 | 0.3078 (7) | 0.0170 (12) | 0.1095 (3) | 0.076 (4)* | 0.5 |
H236 | 0.2859 | 0.0495 | 0.1237 | 0.091* | 0.5 |
C237 | 0.3240 (11) | −0.2742 (18) | 0.0817 (6) | 0.134 (7)* | 0.5 |
H23A | 0.357 | −0.307 | 0.0727 | 0.201* | 0.5 |
H23B | 0.2818 | −0.2882 | 0.0676 | 0.201* | 0.5 |
H23C | 0.326 | −0.3059 | 0.1026 | 0.201* | 0.5 |
O25 | 0.2926 (6) | −0.1144 (10) | 0.1198 (3) | 0.104 (3)* | 0.5 |
C251 | 0.3143 (5) | −0.0379 (8) | 0.1035 (2) | 0.048 (2)* | 0.5 |
C252 | 0.3404 (5) | −0.0829 (7) | 0.0801 (2) | 0.050 (2)* | 0.5 |
C253 | 0.3678 (6) | −0.0120 (9) | 0.0623 (3) | 0.070 (3)* | 0.5 |
H253 | 0.3866 | −0.0391 | 0.0463 | 0.084* | 0.5 |
C254 | 0.3674 (6) | 0.0983 (9) | 0.0681 (3) | 0.078 (3)* | 0.5 |
H254 | 0.3863 | 0.1464 | 0.056 | 0.094* | 0.5 |
C255 | 0.3396 (6) | 0.1405 (10) | 0.0916 (3) | 0.075 (3)* | 0.5 |
H255 | 0.3404 | 0.2164 | 0.0956 | 0.09* | 0.5 |
C256 | 0.3111 (6) | 0.0713 (9) | 0.1089 (3) | 0.066 (3)* | 0.5 |
H256 | 0.2899 | 0.0982 | 0.1241 | 0.079* | 0.5 |
C257 | 0.3424 (7) | −0.2038 (12) | 0.0751 (3) | 0.074 (3)* | 0.5 |
H25A | 0.3785 | −0.2218 | 0.0661 | 0.112* | 0.5 |
H25B | 0.3025 | −0.2273 | 0.0605 | 0.112* | 0.5 |
H25C | 0.3474 | −0.241 | 0.0955 | 0.112* | 0.5 |
P3 | 0.16286 (6) | 0.12118 (9) | 0.17181 (3) | 0.0470 (3) | |
O31 | 0.21613 (16) | 0.2161 (3) | 0.18060 (9) | 0.0544 (8) | |
C311 | 0.2803 (2) | 0.2064 (4) | 0.18050 (12) | 0.0515 (11) | |
C312 | 0.3070 (3) | 0.2956 (4) | 0.16922 (15) | 0.0647 (14) | |
C313 | 0.3713 (3) | 0.2905 (5) | 0.16969 (19) | 0.082 (2) | |
H313 | 0.3908 | 0.3505 | 0.1621 | 0.099* | |
C314 | 0.4079 (3) | 0.1999 (5) | 0.18096 (18) | 0.0797 (19) | |
H314 | 0.4516 | 0.1973 | 0.1805 | 0.096* | |
C315 | 0.3803 (3) | 0.1134 (4) | 0.19291 (15) | 0.0646 (15) | |
H315 | 0.4054 | 0.0518 | 0.2012 | 0.077* | |
C316 | 0.3161 (3) | 0.1166 (4) | 0.19284 (13) | 0.0551 (12) | |
H316 | 0.2969 | 0.0577 | 0.2012 | 0.066* | |
C317 | 0.2669 (3) | 0.3949 (5) | 0.15789 (18) | 0.0779 (18) | |
H31A | 0.2322 | 0.3757 | 0.1395 | 0.117* | |
H31B | 0.2936 | 0.4512 | 0.1518 | 0.117* | |
H31C | 0.2487 | 0.422 | 0.175 | 0.117* | |
O32 | 0.17334 (16) | 0.0753 (3) | 0.20817 (8) | 0.0542 (8) | |
C321 | 0.1375 (3) | −0.0127 (4) | 0.21457 (14) | 0.0587 (13) | |
C322 | 0.1707 (3) | −0.0944 (4) | 0.23422 (13) | 0.0611 (14) | |
C323 | 0.1337 (4) | −0.1801 (5) | 0.24155 (17) | 0.078 (2) | |
H323 | 0.1544 | −0.2368 | 0.255 | 0.094* | |
C324 | 0.0686 (4) | −0.1845 (5) | 0.2298 (2) | 0.095 (3) | |
H324 | 0.0452 | −0.2443 | 0.2349 | 0.114* | |
C325 | 0.0379 (4) | −0.1031 (6) | 0.2111 (2) | 0.100 (3) | |
H325 | −0.0072 | −0.1057 | 0.2031 | 0.12* | |
C326 | 0.0725 (3) | −0.0160 (5) | 0.20359 (19) | 0.0785 (19) | |
H326 | 0.0509 | 0.0414 | 0.1908 | 0.094* | |
C327 | 0.2406 (3) | −0.0898 (5) | 0.24717 (13) | 0.0674 (15) | |
H32A | 0.2621 | −0.1034 | 0.2301 | 0.101* | |
H32B | 0.2535 | −0.145 | 0.2637 | 0.101* | |
H32C | 0.2526 | −0.0178 | 0.2563 | 0.101* | |
O33 | 0.10088 (16) | 0.1985 (2) | 0.16775 (7) | 0.0484 (8) | |
C331 | 0.0935 (2) | 0.2915 (4) | 0.18534 (12) | 0.0470 (11) | |
C332 | 0.0728 (4) | 0.3820 (5) | 0.16820 (15) | 0.084 (2) | |
C333 | 0.0619 (5) | 0.4740 (6) | 0.18498 (18) | 0.109 (3) | |
H333 | 0.0476 | 0.5386 | 0.1735 | 0.13* | |
C334 | 0.0710 (4) | 0.4743 (6) | 0.21727 (17) | 0.084 (2) | |
H334 | 0.0641 | 0.5384 | 0.2281 | 0.101* | |
C335 | 0.0903 (3) | 0.3808 (6) | 0.23366 (14) | 0.0765 (19) | |
H335 | 0.0959 | 0.3789 | 0.2561 | 0.092* | |
C336 | 0.1017 (3) | 0.2887 (5) | 0.21771 (12) | 0.0593 (13) | |
H336 | 0.1151 | 0.2237 | 0.2291 | 0.071* | |
C337 | 0.0616 (6) | 0.3832 (7) | 0.13258 (18) | 0.144 (4) | |
H33A | 0.0919 | 0.3341 | 0.1262 | 0.216* | |
H33B | 0.0677 | 0.457 | 0.1255 | 0.216* | |
H33C | 0.0178 | 0.3594 | 0.1229 | 0.216* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0747 (6) | 0.0502 (5) | 0.0595 (6) | 0.0233 (4) | −0.0109 (5) | −0.0147 (4) |
P1 | 0.0483 (7) | 0.0599 (8) | 0.0532 (7) | 0.0110 (6) | 0.0029 (6) | −0.0140 (6) |
O12 | 0.053 (2) | 0.055 (2) | 0.0511 (19) | 0.0028 (16) | 0.0041 (15) | −0.0056 (15) |
C121 | 0.056 (3) | 0.063 (3) | 0.052 (3) | −0.010 (2) | 0.009 (2) | 0.004 (2) |
C122 | 0.075 (4) | 0.096 (5) | 0.062 (4) | −0.028 (4) | 0.009 (3) | −0.013 (3) |
C123 | 0.114 (7) | 0.173 (9) | 0.082 (5) | −0.081 (7) | 0.025 (5) | −0.024 (6) |
C124 | 0.099 (6) | 0.185 (10) | 0.081 (5) | −0.070 (6) | 0.027 (4) | −0.012 (6) |
C125 | 0.093 (5) | 0.139 (7) | 0.061 (4) | −0.035 (5) | 0.027 (4) | −0.007 (4) |
C126 | 0.064 (3) | 0.074 (4) | 0.056 (3) | −0.006 (3) | 0.008 (3) | −0.004 (3) |
C127 | 0.084 (5) | 0.134 (7) | 0.083 (5) | −0.031 (5) | 0.002 (4) | −0.042 (5) |
O13 | 0.067 (2) | 0.060 (2) | 0.0487 (19) | −0.0053 (17) | 0.0107 (16) | −0.0033 (16) |
C131 | 0.084 (4) | 0.059 (3) | 0.057 (3) | −0.009 (3) | 0.022 (3) | −0.005 (3) |
C132 | 0.088 (5) | 0.111 (6) | 0.073 (4) | −0.034 (4) | 0.014 (4) | 0.001 (4) |
C133 | 0.113 (7) | 0.124 (7) | 0.089 (5) | −0.032 (5) | 0.024 (5) | 0.022 (5) |
C134 | 0.111 (6) | 0.098 (6) | 0.071 (4) | −0.014 (5) | 0.023 (4) | 0.008 (4) |
C135 | 0.095 (5) | 0.074 (4) | 0.075 (4) | 0.004 (4) | 0.012 (4) | 0.009 (3) |
C136 | 0.081 (4) | 0.058 (3) | 0.063 (3) | 0.006 (3) | 0.018 (3) | 0.003 (3) |
C137 | 0.091 (6) | 0.185 (11) | 0.117 (7) | −0.055 (7) | 0.013 (5) | 0.023 (7) |
P2 | 0.041 (3) | 0.048 (2) | 0.044 (2) | 0.0034 (17) | 0.0107 (16) | −0.0104 (16) |
P2' | 0.058 (4) | 0.045 (3) | 0.055 (3) | 0.018 (2) | 0.007 (2) | −0.0050 (18) |
O21 | 0.0491 (18) | 0.0452 (18) | 0.0496 (18) | 0.0076 (14) | 0.0144 (14) | 0.0005 (14) |
C211 | 0.046 (3) | 0.052 (3) | 0.047 (3) | 0.010 (2) | 0.009 (2) | −0.003 (2) |
C212 | 0.072 (4) | 0.053 (3) | 0.067 (3) | 0.018 (3) | 0.031 (3) | 0.005 (3) |
C213 | 0.112 (6) | 0.073 (4) | 0.060 (3) | 0.044 (4) | 0.030 (3) | 0.014 (3) |
C214 | 0.080 (5) | 0.107 (6) | 0.076 (4) | 0.049 (4) | −0.005 (4) | −0.015 (4) |
C215 | 0.042 (3) | 0.125 (7) | 0.130 (7) | 0.016 (4) | 0.005 (4) | −0.040 (6) |
C216 | 0.047 (3) | 0.077 (4) | 0.086 (4) | −0.001 (3) | 0.012 (3) | −0.014 (3) |
C217 | 0.109 (6) | 0.057 (4) | 0.184 (9) | 0.018 (4) | 0.096 (6) | 0.023 (5) |
P3 | 0.0531 (7) | 0.0338 (6) | 0.0487 (7) | 0.0011 (5) | 0.0022 (5) | 0.0010 (5) |
O31 | 0.057 (2) | 0.0375 (17) | 0.068 (2) | −0.0029 (15) | 0.0149 (17) | −0.0048 (15) |
C311 | 0.053 (3) | 0.043 (3) | 0.057 (3) | −0.004 (2) | 0.010 (2) | −0.004 (2) |
C312 | 0.070 (4) | 0.047 (3) | 0.077 (4) | 0.005 (3) | 0.019 (3) | 0.012 (3) |
C313 | 0.064 (4) | 0.062 (4) | 0.128 (6) | −0.003 (3) | 0.036 (4) | 0.021 (4) |
C314 | 0.061 (4) | 0.061 (4) | 0.119 (6) | 0.001 (3) | 0.026 (4) | 0.010 (4) |
C315 | 0.056 (3) | 0.046 (3) | 0.086 (4) | −0.001 (2) | 0.005 (3) | −0.003 (3) |
C316 | 0.060 (3) | 0.036 (2) | 0.067 (3) | −0.006 (2) | 0.011 (2) | −0.004 (2) |
C317 | 0.081 (4) | 0.056 (3) | 0.101 (5) | 0.005 (3) | 0.030 (4) | 0.023 (3) |
O32 | 0.058 (2) | 0.0459 (18) | 0.0530 (19) | 0.0013 (15) | 0.0024 (15) | 0.0090 (15) |
C321 | 0.065 (3) | 0.045 (3) | 0.070 (3) | 0.008 (2) | 0.023 (3) | 0.015 (2) |
C322 | 0.079 (4) | 0.053 (3) | 0.060 (3) | 0.023 (3) | 0.033 (3) | 0.014 (2) |
C323 | 0.104 (5) | 0.052 (3) | 0.097 (5) | 0.028 (3) | 0.059 (4) | 0.030 (3) |
C324 | 0.096 (5) | 0.060 (4) | 0.155 (7) | 0.016 (4) | 0.081 (5) | 0.033 (4) |
C325 | 0.074 (4) | 0.062 (4) | 0.175 (8) | 0.011 (3) | 0.053 (5) | 0.029 (5) |
C326 | 0.065 (4) | 0.049 (3) | 0.125 (6) | 0.010 (3) | 0.030 (4) | 0.025 (3) |
C327 | 0.085 (4) | 0.065 (3) | 0.050 (3) | 0.026 (3) | 0.012 (3) | 0.014 (3) |
O33 | 0.0554 (19) | 0.0374 (17) | 0.0475 (17) | 0.0032 (14) | 0.0032 (14) | −0.0003 (13) |
C331 | 0.046 (3) | 0.041 (2) | 0.054 (3) | −0.0001 (19) | 0.012 (2) | −0.002 (2) |
C332 | 0.152 (7) | 0.048 (3) | 0.057 (3) | 0.026 (4) | 0.038 (4) | 0.005 (3) |
C333 | 0.201 (10) | 0.051 (4) | 0.080 (5) | 0.041 (5) | 0.047 (5) | 0.000 (3) |
C334 | 0.101 (5) | 0.075 (4) | 0.076 (4) | 0.025 (4) | 0.021 (4) | −0.023 (3) |
C335 | 0.068 (4) | 0.106 (5) | 0.053 (3) | 0.030 (4) | 0.010 (3) | −0.012 (3) |
C336 | 0.056 (3) | 0.070 (3) | 0.049 (3) | 0.014 (3) | 0.007 (2) | 0.003 (2) |
C337 | 0.283 (12) | 0.084 (5) | 0.069 (4) | 0.093 (7) | 0.051 (6) | 0.021 (4) |
Ni1—P2 | 2.068 (8) | C225—H225 | 0.95 |
Ni1—P3 | 2.0915 (15) | C226—H226 | 0.95 |
Ni1—P1 | 2.1021 (17) | C227—H22A | 0.98 |
Ni1—P2' | 2.179 (7) | C227—H22B | 0.98 |
P1—O11 | 1.531 (8) | C227—H22C | 0.98 |
P1—O12 | 1.622 (4) | O24—C241 | 1.409 (14) |
P1—O13 | 1.631 (4) | C241—C246 | 1.382 (15) |
P1—O41 | 1.738 (8) | C241—C242 | 1.407 (15) |
O11—C111 | 1.397 (13) | C242—C247 | 1.29 (3) |
C111—C112 | 1.368 (13) | C242—C243 | 1.406 (15) |
C111—C116 | 1.394 (12) | C243—C244 | 1.291 (15) |
C112—C113 | 1.411 (14) | C243—H243 | 0.95 |
C112—C117 | 1.57 (2) | C244—C245 | 1.406 (16) |
C113—C114 | 1.394 (15) | C244—H244 | 0.95 |
C113—H113 | 0.95 | C245—C246 | 1.412 (16) |
C114—C115 | 1.378 (14) | C245—H245 | 0.95 |
C114—H114 | 0.95 | C246—H246 | 0.95 |
C115—C116 | 1.395 (13) | C247—H24A | 0.98 |
C115—H115 | 0.95 | C247—H24B | 0.98 |
C116—H116 | 0.95 | C247—H24C | 0.98 |
C117—H11A | 0.98 | O23—C231 | 1.345 (13) |
C117—H11B | 0.98 | C231—C236 | 1.344 (14) |
C117—H11C | 0.98 | C231—C232 | 1.418 (14) |
O41—C141 | 1.382 (11) | C232—C233 | 1.392 (15) |
C141—C142 | 1.371 (12) | C232—C237 | 1.58 (3) |
C141—C146 | 1.382 (12) | C233—C234 | 1.343 (15) |
C142—C143 | 1.386 (12) | C233—H233 | 0.95 |
C142—C147 | 1.586 (17) | C234—C235 | 1.424 (15) |
C143—C144 | 1.432 (13) | C234—H234 | 0.95 |
C143—H143 | 0.95 | C235—C236 | 1.388 (14) |
C144—C145 | 1.332 (13) | C235—H235 | 0.95 |
C144—H144 | 0.95 | C236—H236 | 0.95 |
C145—C146 | 1.393 (12) | C237—H23A | 0.98 |
C145—H145 | 0.95 | C237—H23B | 0.98 |
C146—H146 | 0.95 | C237—H23C | 0.98 |
C147—H14A | 0.98 | O25—C251 | 1.333 (13) |
C147—H14B | 0.98 | C251—C256 | 1.371 (12) |
C147—H14C | 0.98 | C251—C252 | 1.392 (11) |
O12—C121 | 1.388 (6) | C252—C253 | 1.388 (12) |
C121—C126 | 1.368 (8) | C252—C257 | 1.508 (17) |
C121—C122 | 1.395 (8) | C253—C254 | 1.383 (13) |
C122—C123 | 1.401 (10) | C253—H253 | 0.95 |
C122—C127 | 1.520 (10) | C254—C255 | 1.405 (13) |
C123—C124 | 1.372 (12) | C254—H254 | 0.95 |
C123—H123 | 0.95 | C255—C256 | 1.376 (13) |
C124—C125 | 1.375 (11) | C255—H255 | 0.95 |
C124—H124 | 0.95 | C256—H256 | 0.95 |
C125—C126 | 1.399 (9) | C257—H25A | 0.98 |
C125—H125 | 0.95 | C257—H25B | 0.98 |
C126—H126 | 0.95 | C257—H25C | 0.98 |
C127—H12A | 0.98 | P3—O33 | 1.617 (3) |
C127—H12B | 0.98 | P3—O31 | 1.620 (3) |
C127—H12C | 0.98 | P3—O32 | 1.639 (3) |
O13—C131 | 1.418 (7) | O31—C311 | 1.393 (6) |
C131—C132 | 1.358 (9) | C311—C316 | 1.381 (7) |
C131—C136 | 1.389 (9) | C311—C312 | 1.385 (7) |
C132—C133 | 1.413 (11) | C312—C313 | 1.383 (8) |
C132—C137 | 1.492 (11) | C312—C317 | 1.511 (8) |
C133—C134 | 1.363 (12) | C313—C314 | 1.386 (9) |
C133—H133 | 0.95 | C313—H313 | 0.95 |
C134—C135 | 1.355 (10) | C314—C315 | 1.382 (8) |
C134—H134 | 0.95 | C314—H314 | 0.95 |
C135—C136 | 1.387 (9) | C315—C316 | 1.386 (8) |
C135—H135 | 0.95 | C315—H315 | 0.95 |
C136—H136 | 0.95 | C316—H316 | 0.95 |
C137—H13A | 0.98 | C317—H31A | 0.98 |
C137—H13B | 0.98 | C317—H31B | 0.98 |
C137—H13C | 0.98 | C317—H31C | 0.98 |
P2—O22 | 1.579 (9) | O32—C321 | 1.399 (6) |
P2—O21 | 1.599 (8) | C321—C326 | 1.369 (9) |
P2—O23 | 1.668 (8) | C321—C322 | 1.398 (7) |
P2'—O25 | 1.568 (14) | C322—C323 | 1.406 (8) |
P2'—O24 | 1.593 (15) | C322—C327 | 1.478 (9) |
P2'—O21 | 1.627 (9) | C323—C324 | 1.373 (11) |
O21—C211 | 1.408 (5) | C323—H323 | 0.95 |
C211—C212 | 1.358 (7) | C324—C325 | 1.359 (10) |
C211—C216 | 1.376 (8) | C324—H324 | 0.95 |
C212—C213 | 1.398 (8) | C325—C326 | 1.392 (9) |
C212—C217 | 1.491 (8) | C325—H325 | 0.95 |
C213—C214 | 1.339 (11) | C326—H326 | 0.95 |
C213—H213 | 0.95 | C327—H32A | 0.98 |
C214—C215 | 1.374 (12) | C327—H32B | 0.98 |
C214—H214 | 0.95 | C327—H32C | 0.98 |
C215—C216 | 1.372 (10) | O33—C331 | 1.407 (6) |
C215—H215 | 0.95 | C331—C332 | 1.355 (7) |
C216—H216 | 0.95 | C331—C336 | 1.373 (7) |
C217—H21A | 0.98 | C332—C333 | 1.400 (8) |
C217—H21B | 0.98 | C332—C337 | 1.505 (9) |
C217—H21C | 0.98 | C333—C334 | 1.366 (10) |
O22—C221 | 1.367 (10) | C333—H333 | 0.95 |
C221—C222 | 1.387 (12) | C334—C335 | 1.366 (10) |
C221—C226 | 1.396 (13) | C334—H334 | 0.95 |
C222—C223 | 1.413 (13) | C335—C336 | 1.382 (8) |
C222—C227 | 1.505 (19) | C335—H335 | 0.95 |
C223—C224 | 1.328 (14) | C336—H336 | 0.95 |
C223—H223 | 0.95 | C337—H33A | 0.98 |
C224—C225 | 1.397 (14) | C337—H33B | 0.98 |
C224—H224 | 0.95 | C337—H33C | 0.98 |
C225—C226 | 1.345 (13) | ||
P2—Ni1—P3 | 119.4 (2) | C224—C225—H225 | 120.5 |
P2—Ni1—P1 | 123.1 (2) | C225—C226—C221 | 120.6 (10) |
P3—Ni1—P1 | 115.03 (6) | C225—C226—H226 | 119.7 |
P3—Ni1—P2' | 120.8 (2) | C221—C226—H226 | 119.7 |
P1—Ni1—P2' | 116.0 (2) | C222—C227—H22A | 109.5 |
O11—P1—O12 | 92.7 (3) | C222—C227—H22B | 109.5 |
O11—P1—O13 | 104.7 (4) | H22A—C227—H22B | 109.5 |
O12—P1—O13 | 102.74 (19) | C222—C227—H22C | 109.5 |
O12—P1—O41 | 96.1 (3) | H22A—C227—H22C | 109.5 |
O13—P1—O41 | 86.6 (3) | H22B—C227—H22C | 109.5 |
O11—P1—Ni1 | 117.1 (3) | C241—O24—P2' | 125.1 (12) |
O12—P1—Ni1 | 123.80 (16) | C246—C241—C242 | 123.5 (12) |
O13—P1—Ni1 | 112.65 (14) | C246—C241—O24 | 132.1 (16) |
O41—P1—Ni1 | 127.2 (3) | C242—C241—O24 | 104.4 (14) |
C111—O11—P1 | 132.8 (8) | C247—C242—C243 | 110.0 (19) |
C112—C111—C116 | 122.6 (10) | C247—C242—C241 | 133.0 (19) |
C112—C111—O11 | 116.3 (11) | C243—C242—C241 | 116.9 (12) |
C116—C111—O11 | 121.0 (8) | C244—C243—C242 | 118.2 (13) |
C111—C112—C113 | 120.0 (11) | C244—C243—H243 | 120.9 |
C111—C112—C117 | 119.5 (12) | C242—C243—H243 | 120.9 |
C113—C112—C117 | 120.1 (12) | C243—C244—C245 | 127.8 (13) |
C114—C113—C112 | 115.9 (11) | C243—C244—H244 | 116.1 |
C114—C113—H113 | 122.1 | C245—C244—H244 | 116.1 |
C112—C113—H113 | 122.1 | C244—C245—C246 | 115.3 (13) |
C115—C114—C113 | 124.5 (12) | C244—C245—H245 | 122.3 |
C115—C114—H114 | 117.8 | C246—C245—H245 | 122.3 |
C113—C114—H114 | 117.8 | C241—C246—C245 | 117.8 (13) |
C114—C115—C116 | 118.0 (11) | C241—C246—H246 | 121.1 |
C114—C115—H115 | 121 | C245—C246—H246 | 121.1 |
C116—C115—H115 | 121 | C242—C247—H24A | 109.5 |
C111—C116—C115 | 118.5 (9) | C242—C247—H24B | 109.5 |
C111—C116—H116 | 120.8 | H24A—C247—H24B | 109.5 |
C115—C116—H116 | 120.8 | C242—C247—H24C | 109.5 |
C112—C117—H11A | 109.5 | H24A—C247—H24C | 109.5 |
C112—C117—H11B | 109.5 | H24B—C247—H24C | 109.5 |
H11A—C117—H11B | 109.5 | C231—O23—P2 | 129.3 (8) |
C112—C117—H11C | 109.5 | C236—C231—O23 | 122.9 (11) |
H11A—C117—H11C | 109.5 | C236—C231—C232 | 123.5 (11) |
H11B—C117—H11C | 109.5 | O23—C231—C232 | 113.4 (12) |
C141—O41—P1 | 120.7 (7) | C233—C232—C231 | 113.8 (12) |
C142—C141—O41 | 116.3 (9) | C233—C232—C237 | 128.7 (16) |
C142—C141—C146 | 119.8 (8) | C231—C232—C237 | 117.5 (15) |
O41—C141—C146 | 123.8 (8) | C234—C233—C232 | 123.3 (13) |
C141—C142—C143 | 120.2 (10) | C234—C233—H233 | 118.3 |
C141—C142—C147 | 117.7 (9) | C232—C233—H233 | 118.3 |
C143—C142—C147 | 121.8 (10) | C233—C234—C235 | 121.8 (13) |
C142—C143—C144 | 118.0 (9) | C233—C234—H234 | 119.1 |
C142—C143—H143 | 121 | C235—C234—H234 | 119.1 |
C144—C143—H143 | 121 | C236—C235—C234 | 115.1 (12) |
C145—C144—C143 | 121.2 (10) | C236—C235—H235 | 122.4 |
C145—C144—H144 | 119.4 | C234—C235—H235 | 122.4 |
C143—C144—H144 | 119.4 | C231—C236—C235 | 121.9 (12) |
C144—C145—C146 | 119.2 (10) | C231—C236—H236 | 119 |
C144—C145—H145 | 120.4 | C235—C236—H236 | 119 |
C146—C145—H145 | 120.4 | C232—C237—H23A | 109.5 |
C141—C146—C145 | 120.7 (9) | C232—C237—H23B | 109.5 |
C141—C146—H146 | 119.7 | H23A—C237—H23B | 109.5 |
C145—C146—H146 | 119.7 | C232—C237—H23C | 109.5 |
C142—C147—H14A | 109.5 | H23A—C237—H23C | 109.5 |
C142—C147—H14B | 109.5 | H23B—C237—H23C | 109.5 |
H14A—C147—H14B | 109.5 | C251—O25—P2' | 128.3 (10) |
C142—C147—H14C | 109.5 | O25—C251—C256 | 124.4 (10) |
H14A—C147—H14C | 109.5 | O25—C251—C252 | 111.4 (10) |
H14B—C147—H14C | 109.5 | C256—C251—C252 | 124.3 (8) |
C121—O12—P1 | 125.9 (3) | C253—C252—C251 | 117.1 (8) |
C126—C121—O12 | 122.4 (5) | C253—C252—C257 | 120.9 (9) |
C126—C121—C122 | 122.6 (6) | C251—C252—C257 | 121.9 (9) |
O12—C121—C122 | 115.0 (5) | C254—C253—C252 | 119.8 (9) |
C121—C122—C123 | 116.4 (6) | C254—C253—H253 | 120.1 |
C121—C122—C127 | 121.5 (6) | C252—C253—H253 | 120.1 |
C123—C122—C127 | 122.0 (6) | C253—C254—C255 | 121.3 (10) |
C124—C123—C122 | 121.9 (7) | C253—C254—H254 | 119.4 |
C124—C123—H123 | 119 | C255—C254—H254 | 119.4 |
C122—C123—H123 | 119 | C256—C255—C254 | 119.5 (10) |
C123—C124—C125 | 120.1 (8) | C256—C255—H255 | 120.2 |
C123—C124—H124 | 119.9 | C254—C255—H255 | 120.2 |
C125—C124—H124 | 119.9 | C251—C256—C255 | 117.9 (9) |
C124—C125—C126 | 119.7 (7) | C251—C256—H256 | 121.1 |
C124—C125—H125 | 120.1 | C255—C256—H256 | 121.1 |
C126—C125—H125 | 120.1 | C252—C257—H25A | 109.5 |
C121—C126—C125 | 119.2 (6) | C252—C257—H25B | 109.5 |
C121—C126—H126 | 120.4 | H25A—C257—H25B | 109.5 |
C125—C126—H126 | 120.4 | C252—C257—H25C | 109.5 |
C122—C127—H12A | 109.5 | H25A—C257—H25C | 109.5 |
C122—C127—H12B | 109.5 | H25B—C257—H25C | 109.5 |
H12A—C127—H12B | 109.5 | O33—P3—O31 | 96.93 (18) |
C122—C127—H12C | 109.5 | O33—P3—O32 | 102.99 (18) |
H12A—C127—H12C | 109.5 | O31—P3—O32 | 95.72 (19) |
H12B—C127—H12C | 109.5 | O33—P3—Ni1 | 116.00 (13) |
C131—O13—P1 | 124.7 (3) | O31—P3—Ni1 | 120.88 (15) |
C132—C131—C136 | 122.2 (6) | O32—P3—Ni1 | 119.98 (14) |
C132—C131—O13 | 118.2 (6) | C311—O31—P3 | 126.0 (3) |
C136—C131—O13 | 119.6 (5) | C316—C311—C312 | 122.2 (5) |
C131—C132—C133 | 117.0 (7) | C316—C311—O31 | 122.0 (5) |
C131—C132—C137 | 120.8 (7) | C312—C311—O31 | 115.7 (5) |
C133—C132—C137 | 122.2 (7) | C313—C312—C311 | 117.4 (5) |
C134—C133—C132 | 121.3 (7) | C313—C312—C317 | 122.4 (5) |
C134—C133—H133 | 119.3 | C311—C312—C317 | 120.2 (5) |
C132—C133—H133 | 119.3 | C312—C313—C314 | 121.7 (6) |
C135—C134—C133 | 120.4 (8) | C312—C313—H313 | 119.2 |
C135—C134—H134 | 119.8 | C314—C313—H313 | 119.2 |
C133—C134—H134 | 119.8 | C315—C314—C313 | 119.6 (6) |
C134—C135—C136 | 120.1 (7) | C315—C314—H314 | 120.2 |
C134—C135—H135 | 120 | C313—C314—H314 | 120.2 |
C136—C135—H135 | 120 | C314—C315—C316 | 119.9 (5) |
C135—C136—C131 | 119.0 (6) | C314—C315—H315 | 120 |
C135—C136—H136 | 120.5 | C316—C315—H315 | 120 |
C131—C136—H136 | 120.5 | C311—C316—C315 | 119.2 (5) |
C132—C137—H13A | 109.5 | C311—C316—H316 | 120.4 |
C132—C137—H13B | 109.5 | C315—C316—H316 | 120.4 |
H13A—C137—H13B | 109.5 | C312—C317—H31A | 109.5 |
C132—C137—H13C | 109.5 | C312—C317—H31B | 109.5 |
H13A—C137—H13C | 109.5 | H31A—C317—H31B | 109.5 |
H13B—C137—H13C | 109.5 | C312—C317—H31C | 109.5 |
O22—P2—O21 | 98.9 (5) | H31A—C317—H31C | 109.5 |
O22—P2—O23 | 92.4 (5) | H31B—C317—H31C | 109.5 |
O21—P2—O23 | 99.0 (4) | C321—O32—P3 | 120.4 (3) |
O22—P2—Ni1 | 121.7 (4) | C326—C321—C322 | 121.3 (5) |
O21—P2—Ni1 | 120.5 (4) | C326—C321—O32 | 121.6 (5) |
O23—P2—Ni1 | 118.6 (4) | C322—C321—O32 | 117.1 (5) |
O25—P2'—O24 | 89.3 (8) | C321—C322—C323 | 116.4 (6) |
O25—P2'—O21 | 101.5 (6) | C321—C322—C327 | 121.8 (5) |
O24—P2'—O21 | 101.0 (6) | C323—C322—C327 | 121.8 (5) |
O25—P2'—Ni1 | 131.4 (6) | C324—C323—C322 | 122.1 (6) |
O24—P2'—Ni1 | 114.8 (6) | C324—C323—H323 | 118.9 |
O21—P2'—Ni1 | 113.2 (4) | C322—C323—H323 | 118.9 |
C211—O21—P2 | 127.5 (4) | C325—C324—C323 | 120.0 (6) |
C211—O21—P2' | 123.7 (4) | C325—C324—H324 | 120 |
C212—C211—C216 | 121.0 (5) | C323—C324—H324 | 120 |
C212—C211—O21 | 120.8 (4) | C324—C325—C326 | 119.8 (7) |
C216—C211—O21 | 117.9 (5) | C324—C325—H325 | 120.1 |
C211—C212—C213 | 117.9 (6) | C326—C325—H325 | 120.1 |
C211—C212—C217 | 123.5 (5) | C321—C326—C325 | 120.4 (6) |
C213—C212—C217 | 118.6 (6) | C321—C326—H326 | 119.8 |
C214—C213—C212 | 122.2 (7) | C325—C326—H326 | 119.8 |
C214—C213—H213 | 118.9 | C322—C327—H32A | 109.5 |
C212—C213—H213 | 118.9 | C322—C327—H32B | 109.5 |
C213—C214—C215 | 119.0 (6) | H32A—C327—H32B | 109.5 |
C213—C214—H214 | 120.5 | C322—C327—H32C | 109.5 |
C215—C214—H214 | 120.5 | H32A—C327—H32C | 109.5 |
C216—C215—C214 | 120.6 (7) | H32B—C327—H32C | 109.5 |
C216—C215—H215 | 119.7 | C331—O33—P3 | 128.4 (3) |
C214—C215—H215 | 119.7 | C332—C331—C336 | 121.6 (5) |
C215—C216—C211 | 119.4 (7) | C332—C331—O33 | 116.0 (4) |
C215—C216—H216 | 120.3 | C336—C331—O33 | 122.1 (4) |
C211—C216—H216 | 120.3 | C331—C332—C333 | 117.2 (6) |
C212—C217—H21A | 109.5 | C331—C332—C337 | 121.4 (5) |
C212—C217—H21B | 109.5 | C333—C332—C337 | 121.4 (6) |
H21A—C217—H21B | 109.5 | C334—C333—C332 | 122.4 (6) |
C212—C217—H21C | 109.5 | C334—C333—H333 | 118.8 |
H21A—C217—H21C | 109.5 | C332—C333—H333 | 118.8 |
H21B—C217—H21C | 109.5 | C335—C334—C333 | 118.8 (6) |
C221—O22—P2 | 115.4 (6) | C335—C334—H334 | 120.6 |
O22—C221—C222 | 117.2 (9) | C333—C334—H334 | 120.6 |
O22—C221—C226 | 120.3 (8) | C334—C335—C336 | 120.1 (6) |
C222—C221—C226 | 122.5 (9) | C334—C335—H335 | 120 |
C221—C222—C223 | 113.2 (9) | C336—C335—H335 | 120 |
C221—C222—C227 | 120.5 (11) | C331—C336—C335 | 119.9 (5) |
C223—C222—C227 | 125.5 (11) | C331—C336—H336 | 120.1 |
C224—C223—C222 | 125.0 (12) | C335—C336—H336 | 120.1 |
C224—C223—H223 | 117.5 | C332—C337—H33A | 109.5 |
C222—C223—H223 | 117.5 | C332—C337—H33B | 109.5 |
C223—C224—C225 | 119.1 (12) | H33A—C337—H33B | 109.5 |
C223—C224—H224 | 120.4 | C332—C337—H33C | 109.5 |
C225—C224—H224 | 120.4 | H33A—C337—H33C | 109.5 |
C226—C225—C224 | 119.1 (11) | H33B—C337—H33C | 109.5 |
C226—C225—H225 | 120.5 |
Experimental details
Crystal data | |
Chemical formula | [Ni(C21H21O3P)3] |
Mr | 1115.75 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 100 |
a, b, c (Å) | 21.5898 (9), 12.3292 (3), 43.403 (2) |
β (°) | 104.129 (5) |
V (Å3) | 11203.8 (7) |
Z | 8 |
Radiation type | Cu Kα |
µ (mm−1) | 1.77 |
Crystal size (mm) | 0.28 × 0.11 × 0.07 |
Data collection | |
Diffractometer | Oxford Gemini diffractometer |
Absorption correction | Analytical (CrysAlis PRO; Agilent, 2013) |
Tmin, Tmax | 0.726, 0.896 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 56232, 9993, 8185 |
Rint | 0.043 |
(sin θ/λ)max (Å−1) | 0.599 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.099, 0.259, 1.06 |
No. of reflections | 9993 |
No. of parameters | 682 |
No. of restraints | 82 |
H-atom treatment | H-atom parameters constrained |
w = 1/[σ2(Fo2) + (0.1046P)2 + 70.9791P] where P = (Fo2 + 2Fc2)/3 | |
Δρmax, Δρmin (e Å−3) | 1.26, −1.41 |
Computer programs: CrysAlis PRO (Agilent, 2013), SIR92 (Altomare et al., 1994), SHELXL2014 (Sheldrick, 2015), DIAMOND (Brandenburg, 1999), WinGX (Farrugia, 2012).