Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803021949/ob6309sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803021949/ob6309Isup2.hkl |
CCDC reference: 195285
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.006 Å
- R factor = 0.043
- wR factor = 0.100
- Data-to-parameter ratio = 19.3
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry ..... 95 PerFit PLAT113_ALERT_2_B ADDSYM Suggests Possible Pseudo/New Spacegroup . C2/c PLAT230_ALERT_2_B Hirshfeld Test Diff for O2 - C17 = 9.80 su
Alert level C PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.01 Ratio PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.99 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.02 Ratio PLAT230_ALERT_2_C Hirshfeld Test Diff for C1 - C6 = 5.04 su PLAT230_ALERT_2_C Hirshfeld Test Diff for C11 - C12 = 5.95 su PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors .... C21 PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C23 PLAT411_ALERT_2_C Short Inter H...H Contact H16A .. H22 = 2.14 Ang. PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 3 N1 -NI1 -O1 -C14 111.00 3.00 2.655 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 4 O1 -NI1 -N1 -C8 65.00 3.00 2.655 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 7 O1 -NI1 -N1 -C7 -117.00 3.00 2.655 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 52 N2 -NI2 -O3 -C31 -86.40 1.10 2.656 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 56 O3 -NI2 -N2 -C25 -89.60 1.10 2.656 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 59 O3 -NI2 -N2 -C24 81.80 1.10 2.656 1.555 1.555 1.555 PLAT742_ALERT_1_C Angle Calc 126.1(4), Rep 126.12 ...... Missing su N1 -C8 -C9 1.555 1.555 1.555
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 28.25 From the CIF: _reflns_number_total 7242 Count of symmetry unique reflns 3769 Completeness (_total/calc) 192.15% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 3473 Fraction of Friedel pairs measured 0.921 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 16 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 10 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 8 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: XSCANS (Siemens, 1996); cell refinement: XSCANS; data reduction: SHELXTL (Siemens, 1996); 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.
[Ni(C34H34N2O4)] | Dx = 1.346 Mg m−3 |
Mr = 593.34 | Melting point: 512 K |
Monoclinic, C2 | Mo Kα radiation, λ = 0.71073 Å |
a = 24.101 (3) Å | Cell parameters from 29 reflections |
b = 13.760 (1) Å | θ = 3.0–14.2° |
c = 8.989 (1) Å | µ = 0.70 mm−1 |
β = 100.87 (1)° | T = 295 K |
V = 2927.3 (5) Å3 | Block, brown |
Z = 4 | 0.52 × 0.40 × 0.32 mm |
F(000) = 1248 |
Siemens P4 diffractometer | 5073 reflections with I > 2σ(I) |
Radiation source: normal-focus sealed tube | Rint = 0.014 |
Graphite monochromator | θmax = 28.3°, θmin = 1.7° |
ω scans | h = −32→32 |
Absorption correction: ψ scan (SHELXTL; Siemens, 1996) | k = −18→18 |
Tmin = 0.738, Tmax = 0.798 | l = −11→11 |
7965 measured reflections | 3 standard reflections every 97 reflections |
7242 independent reflections | intensity decay: 2.5% |
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.043 | w = 1/[σ2(Fo2) + (0.0454P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.100 | (Δ/σ)max = 0.001 |
S = 0.96 | Δρmax = 0.47 e Å−3 |
7242 reflections | Δρmin = −0.27 e Å−3 |
376 parameters | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
1 restraint | Extinction coefficient: 0.00045 (13) |
Primary atom site location: structure-invariant direct methods | Absolute structure: Flack (1983), 3473 Friedel pairs |
Secondary atom site location: difference Fourier map | Absolute structure parameter: 0.038 (15) |
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. |
x | y | z | Uiso*/Ueq | ||
Ni1 | 0.5000 | 0.40797 (4) | 0.0000 | 0.03748 (17) | |
O1 | 0.45311 (12) | 0.5061 (2) | 0.0383 (3) | 0.0456 (8) | |
O2 | 0.34447 (15) | 0.7422 (3) | 0.0063 (4) | 0.0870 (11) | |
N1 | 0.45378 (14) | 0.3093 (2) | 0.0494 (4) | 0.0368 (8) | |
C1 | 0.46305 (15) | 0.1038 (3) | 0.2184 (4) | 0.0514 (9) | |
H1 | 0.4874 | 0.1458 | 0.2803 | 0.062* | |
C2 | 0.44399 (17) | 0.0202 (3) | 0.2791 (5) | 0.0664 (11) | |
H2 | 0.4555 | 0.0065 | 0.3816 | 0.080* | |
C3 | 0.4082 (2) | −0.0425 (3) | 0.1883 (6) | 0.0794 (15) | |
H3 | 0.3964 | −0.0996 | 0.2282 | 0.095* | |
C4 | 0.3902 (2) | −0.0204 (3) | 0.0403 (6) | 0.0828 (16) | |
H4 | 0.3648 | −0.0615 | −0.0202 | 0.099* | |
C5 | 0.40903 (17) | 0.0623 (3) | −0.0224 (5) | 0.0613 (10) | |
H5 | 0.3967 | 0.0758 | −0.1247 | 0.074* | |
C6 | 0.44610 (15) | 0.1247 (3) | 0.0665 (4) | 0.0386 (9) | |
C7 | 0.46794 (12) | 0.2120 (2) | −0.0077 (4) | 0.0369 (7) | |
H7 | 0.4516 | 0.2093 | −0.1161 | 0.044* | |
C8 | 0.41316 (18) | 0.3195 (3) | 0.1206 (5) | 0.0414 (10) | |
H8 | 0.3975 | 0.2630 | 0.1516 | 0.050* | |
C9 | 0.38984 (13) | 0.4082 (4) | 0.1567 (4) | 0.0403 (8) | |
C10 | 0.34386 (15) | 0.4051 (4) | 0.2335 (4) | 0.0480 (9) | |
H10 | 0.3337 | 0.3465 | 0.2723 | 0.058* | |
C11 | 0.31377 (19) | 0.4888 (4) | 0.2514 (5) | 0.0591 (13) | |
C12 | 0.32882 (18) | 0.5761 (3) | 0.1846 (4) | 0.0513 (11) | |
H12 | 0.3074 | 0.6317 | 0.1903 | 0.062* | |
C13 | 0.37405 (17) | 0.5810 (3) | 0.1117 (4) | 0.0454 (11) | |
C14 | 0.4080 (2) | 0.4975 (3) | 0.0995 (5) | 0.0440 (11) | |
C15 | 0.2654 (2) | 0.4865 (4) | 0.3362 (5) | 0.0890 (18) | |
H15A | 0.2533 | 0.4205 | 0.3444 | 0.107* | |
H15B | 0.2345 | 0.5243 | 0.2825 | 0.107* | |
H15C | 0.2775 | 0.5131 | 0.4358 | 0.107* | |
C16 | 0.38927 (19) | 0.6745 (3) | 0.0398 (6) | 0.0647 (14) | |
H16A | 0.4205 | 0.7050 | 0.1076 | 0.078* | |
H16B | 0.4022 | 0.6587 | −0.0532 | 0.078* | |
C17 | 0.3089 (2) | 0.7157 (5) | −0.1304 (5) | 0.111 (2) | |
H17A | 0.3312 | 0.7043 | −0.2065 | 0.133* | |
H17B | 0.2825 | 0.7672 | −0.1627 | 0.133* | |
H17C | 0.2887 | 0.6576 | −0.1151 | 0.133* | |
Ni2 | 0.5000 | 0.41741 (3) | 0.5000 | 0.03721 (16) | |
O3 | 0.54490 (12) | 0.31790 (19) | 0.4459 (3) | 0.0431 (7) | |
O4 | 0.65755 (12) | 0.0900 (2) | 0.4908 (3) | 0.0605 (8) | |
N2 | 0.53612 (15) | 0.5161 (2) | 0.4160 (4) | 0.0395 (8) | |
C18 | 0.60015 (18) | 0.7104 (3) | 0.5019 (5) | 0.0682 (12) | |
H18 | 0.6137 | 0.6622 | 0.5720 | 0.082* | |
C19 | 0.6321 (2) | 0.7909 (4) | 0.4920 (5) | 0.0908 (17) | |
H19 | 0.6669 | 0.7972 | 0.5565 | 0.109* | |
C20 | 0.6141 (2) | 0.8622 (4) | 0.3898 (8) | 0.094 (2) | |
H20 | 0.6362 | 0.9171 | 0.3846 | 0.113* | |
C21 | 0.5637 (2) | 0.8521 (4) | 0.2960 (8) | 0.110 (2) | |
H21 | 0.5513 | 0.8997 | 0.2239 | 0.132* | |
C22 | 0.53021 (18) | 0.7710 (3) | 0.3063 (6) | 0.0791 (14) | |
H22 | 0.4953 | 0.7658 | 0.2420 | 0.095* | |
C23 | 0.54741 (17) | 0.6992 (3) | 0.4083 (4) | 0.0452 (10) | |
C24 | 0.51040 (14) | 0.6139 (2) | 0.4254 (4) | 0.0396 (7) | |
H24 | 0.4771 | 0.6179 | 0.3440 | 0.047* | |
C25 | 0.57540 (17) | 0.5054 (3) | 0.3381 (5) | 0.0433 (10) | |
H25 | 0.5855 | 0.5600 | 0.2882 | 0.052* | |
C26 | 0.60486 (14) | 0.4167 (4) | 0.3217 (4) | 0.0420 (8) | |
C27 | 0.65167 (15) | 0.4172 (4) | 0.2493 (4) | 0.0503 (9) | |
H27 | 0.6599 | 0.4747 | 0.2036 | 0.060* | |
C28 | 0.68538 (18) | 0.3404 (3) | 0.2416 (4) | 0.0482 (10) | |
C29 | 0.67137 (17) | 0.2567 (3) | 0.3101 (4) | 0.0504 (11) | |
H29 | 0.6939 | 0.2022 | 0.3067 | 0.060* | |
C30 | 0.62604 (17) | 0.2480 (3) | 0.3836 (4) | 0.0466 (11) | |
C31 | 0.59050 (18) | 0.3294 (3) | 0.3862 (4) | 0.0368 (10) | |
C32 | 0.73431 (18) | 0.3447 (4) | 0.1594 (5) | 0.0704 (15) | |
H32A | 0.7260 | 0.3902 | 0.0773 | 0.085* | |
H32B | 0.7404 | 0.2815 | 0.1202 | 0.085* | |
H32C | 0.7677 | 0.3651 | 0.2283 | 0.085* | |
C33 | 0.61270 (18) | 0.1560 (3) | 0.4595 (5) | 0.0552 (12) | |
H33A | 0.6010 | 0.1727 | 0.5538 | 0.066* | |
H33B | 0.5810 | 0.1243 | 0.3951 | 0.066* | |
C34 | 0.69603 (19) | 0.1142 (4) | 0.6225 (5) | 0.0797 (15) | |
H34A | 0.7100 | 0.1788 | 0.6131 | 0.096* | |
H34B | 0.7270 | 0.0691 | 0.6368 | 0.096* | |
H34C | 0.6775 | 0.1113 | 0.7081 | 0.096* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0341 (3) | 0.0300 (4) | 0.0488 (4) | 0.000 | 0.0088 (3) | 0.000 |
O1 | 0.0424 (17) | 0.0320 (17) | 0.0638 (19) | 0.0014 (14) | 0.0134 (15) | −0.0008 (15) |
O2 | 0.088 (3) | 0.060 (2) | 0.117 (3) | 0.0161 (19) | 0.028 (2) | −0.002 (2) |
N1 | 0.0352 (18) | 0.0282 (15) | 0.0476 (18) | 0.0016 (12) | 0.0094 (15) | 0.0007 (14) |
C1 | 0.047 (2) | 0.044 (2) | 0.067 (2) | 0.0010 (16) | 0.0187 (17) | 0.0036 (18) |
C2 | 0.079 (3) | 0.060 (2) | 0.068 (3) | 0.017 (2) | 0.033 (2) | 0.024 (2) |
C3 | 0.116 (4) | 0.033 (2) | 0.104 (4) | −0.007 (3) | 0.059 (3) | 0.004 (2) |
C4 | 0.113 (4) | 0.050 (3) | 0.097 (4) | −0.038 (3) | 0.050 (3) | −0.017 (3) |
C5 | 0.078 (3) | 0.046 (2) | 0.063 (2) | −0.015 (2) | 0.022 (2) | −0.0048 (19) |
C6 | 0.041 (2) | 0.0281 (19) | 0.050 (2) | 0.0001 (16) | 0.0183 (17) | −0.0016 (15) |
C7 | 0.0403 (17) | 0.0286 (14) | 0.0422 (17) | −0.0022 (13) | 0.0092 (14) | 0.0004 (14) |
C8 | 0.037 (2) | 0.036 (2) | 0.054 (2) | −0.0011 (15) | 0.0153 (18) | 0.0063 (17) |
C9 | 0.0379 (17) | 0.0367 (19) | 0.0470 (18) | 0.007 (2) | 0.0096 (14) | −0.005 (2) |
C10 | 0.0461 (19) | 0.046 (2) | 0.056 (2) | 0.003 (2) | 0.0197 (16) | −0.002 (2) |
C11 | 0.051 (3) | 0.067 (3) | 0.062 (3) | 0.014 (3) | 0.016 (2) | −0.009 (3) |
C12 | 0.056 (3) | 0.041 (2) | 0.057 (3) | 0.013 (2) | 0.011 (2) | −0.002 (2) |
C13 | 0.043 (2) | 0.038 (2) | 0.052 (2) | 0.0098 (19) | −0.001 (2) | −0.0081 (19) |
C14 | 0.043 (2) | 0.037 (2) | 0.049 (3) | 0.002 (2) | 0.002 (2) | −0.004 (2) |
C15 | 0.081 (4) | 0.092 (5) | 0.107 (4) | 0.014 (3) | 0.050 (3) | 0.008 (4) |
C16 | 0.058 (3) | 0.034 (2) | 0.106 (4) | 0.003 (2) | 0.025 (3) | −0.001 (3) |
C17 | 0.095 (4) | 0.164 (7) | 0.068 (3) | −0.028 (5) | −0.002 (3) | −0.004 (4) |
Ni2 | 0.0401 (3) | 0.0271 (3) | 0.0467 (3) | 0.000 | 0.0141 (3) | 0.000 |
O3 | 0.0427 (17) | 0.0289 (15) | 0.0627 (17) | 0.0027 (13) | 0.0225 (15) | −0.0012 (13) |
O4 | 0.071 (2) | 0.0426 (17) | 0.0685 (19) | 0.0153 (15) | 0.0150 (16) | 0.0011 (15) |
N2 | 0.0442 (17) | 0.0311 (16) | 0.0445 (19) | 0.0034 (14) | 0.0118 (14) | 0.0024 (13) |
C18 | 0.076 (3) | 0.075 (3) | 0.054 (2) | −0.027 (2) | 0.011 (2) | 0.007 (2) |
C19 | 0.086 (4) | 0.112 (4) | 0.080 (3) | −0.058 (3) | 0.029 (3) | −0.028 (3) |
C20 | 0.094 (4) | 0.044 (3) | 0.166 (6) | −0.030 (3) | 0.077 (5) | −0.017 (4) |
C21 | 0.091 (4) | 0.047 (3) | 0.202 (7) | 0.005 (3) | 0.054 (4) | 0.053 (4) |
C22 | 0.056 (2) | 0.054 (2) | 0.126 (4) | 0.004 (2) | 0.015 (3) | 0.040 (3) |
C23 | 0.052 (2) | 0.031 (2) | 0.057 (2) | 0.0008 (18) | 0.0210 (19) | −0.0010 (17) |
C24 | 0.0442 (18) | 0.0282 (15) | 0.0465 (18) | −0.0004 (13) | 0.0089 (15) | 0.0006 (14) |
C25 | 0.050 (2) | 0.0335 (19) | 0.048 (2) | 0.0014 (16) | 0.0147 (18) | 0.0056 (16) |
C26 | 0.0451 (19) | 0.041 (2) | 0.0402 (17) | 0.000 (2) | 0.0094 (15) | 0.003 (2) |
C27 | 0.054 (2) | 0.056 (2) | 0.0437 (18) | 0.005 (3) | 0.0155 (17) | 0.009 (3) |
C28 | 0.047 (2) | 0.053 (3) | 0.047 (2) | 0.008 (2) | 0.0148 (19) | 0.003 (2) |
C29 | 0.046 (2) | 0.054 (3) | 0.054 (2) | 0.017 (2) | 0.017 (2) | −0.007 (2) |
C30 | 0.049 (3) | 0.042 (3) | 0.050 (2) | 0.004 (2) | 0.013 (2) | −0.0024 (19) |
C31 | 0.037 (2) | 0.039 (2) | 0.035 (2) | 0.0016 (19) | 0.0086 (17) | −0.0041 (17) |
C32 | 0.062 (3) | 0.080 (4) | 0.080 (3) | 0.021 (3) | 0.041 (3) | 0.010 (3) |
C33 | 0.057 (3) | 0.042 (3) | 0.067 (3) | 0.013 (2) | 0.013 (2) | 0.001 (2) |
C34 | 0.066 (3) | 0.083 (4) | 0.087 (3) | 0.018 (3) | 0.007 (3) | 0.002 (3) |
Ni1—O1i | 1.835 (3) | C25—C26 | 1.434 (6) |
Ni1—O1 | 1.835 (3) | C26—C27 | 1.404 (5) |
Ni1—N1 | 1.862 (3) | C26—C31 | 1.405 (6) |
Ni1—N1i | 1.862 (3) | C27—C28 | 1.343 (6) |
O1—C14 | 1.313 (5) | C28—C29 | 1.378 (6) |
O2—C17 | 1.407 (5) | C28—C32 | 1.506 (5) |
O2—C16 | 1.415 (5) | C29—C30 | 1.384 (5) |
N1—C8 | 1.274 (5) | C30—C31 | 1.413 (6) |
N1—C7 | 1.496 (4) | C30—C33 | 1.502 (6) |
C1—C6 | 1.380 (5) | C1—H1 | 0.930 |
C1—C2 | 1.388 (5) | C2—H2 | 0.930 |
C2—C3 | 1.375 (6) | C3—H3 | 0.930 |
C3—C4 | 1.353 (6) | C4—H4 | 0.930 |
C4—C5 | 1.383 (5) | C5—H5 | 0.930 |
C5—C6 | 1.381 (5) | C7—H7 | 0.980 |
C6—C7 | 1.515 (5) | C8—H8 | 0.930 |
C7—C7i | 1.525 (6) | C10—H10 | 0.930 |
C8—C9 | 1.407 (6) | C12—H12 | 0.930 |
C9—C10 | 1.412 (5) | C15—H15c | 0.960 |
C9—C14 | 1.433 (6) | C15—H15b | 0.961 |
C10—C11 | 1.387 (6) | C15—H15a | 0.961 |
C11—C12 | 1.420 (6) | C16—H16a | 0.970 |
C11—C15 | 1.510 (6) | C16—H16b | 0.970 |
C12—C13 | 1.376 (6) | C17—H17a | 0.959 |
C13—C14 | 1.426 (6) | C17—H17c | 0.959 |
C13—C16 | 1.516 (6) | C17—H17b | 0.960 |
Ni2—N2 | 1.849 (4) | C18—H18 | 0.931 |
Ni2—N2ii | 1.849 (4) | C19—H19 | 0.929 |
Ni2—O3 | 1.866 (3) | C20—H20 | 0.931 |
Ni2—O3ii | 1.866 (3) | C21—H21 | 0.930 |
O3—C31 | 1.320 (5) | C22—H22 | 0.929 |
O4—C33 | 1.399 (4) | C24—H24 | 0.980 |
O4—C34 | 1.399 (5) | C25—H25 | 0.931 |
N2—C25 | 1.288 (5) | C27—H27 | 0.930 |
N2—C24 | 1.491 (4) | C29—H29 | 0.930 |
C18—C19 | 1.362 (6) | C32—H32a | 0.960 |
C18—C23 | 1.394 (5) | C32—H32b | 0.960 |
C19—C20 | 1.358 (7) | C32—H32c | 0.960 |
C20—C21 | 1.350 (7) | C33—H33a | 0.970 |
C21—C22 | 1.391 (6) | C33—H33b | 0.971 |
C22—C23 | 1.358 (5) | C34—H34a | 0.960 |
C23—C24 | 1.500 (5) | C34—H34b | 0.961 |
C24—C24ii | 1.518 (6) | C34—H34c | 0.961 |
O1i—Ni1—O1 | 85.22 (18) | O4—C33—C30 | 114.5 (4) |
O1i—Ni1—N1 | 177.07 (17) | H1—C1—C6 | 119.88 |
O1—Ni1—N1 | 94.26 (11) | H1—C1—C2 | 119.88 |
O1i—Ni1—N1i | 94.26 (11) | H2—C2—C3 | 119.84 |
O1—Ni1—N1i | 177.07 (17) | H2—C2—C1 | 119.90 |
N1—Ni1—N1i | 86.4 (2) | H3—C3—C4 | 120.26 |
C14—O1—Ni1 | 126.9 (3) | H3—C3—C2 | 120.30 |
C17—O2—C16 | 109.3 (4) | H4—C4—C3 | 119.45 |
C8—N1—C7 | 121.2 (3) | H4—C4—C5 | 119.48 |
C8—N1—Ni1 | 126.2 (3) | H5—C5—C6 | 119.96 |
C7—N1—Ni1 | 112.6 (2) | H5—C5—C4 | 119.91 |
C6—C1—C2 | 120.3 (4) | H7—C7—N1 | 107.46 |
C3—C2—C1 | 120.2 (4) | H7—C7—C6 | 107.43 |
C4—C3—C2 | 119.4 (4) | H7—C7—C7i | 107.48 |
C3—C4—C5 | 121.1 (4) | H8—C8—N1 | 116.89 |
C6—C5—C4 | 120.1 (4) | H8—C8—C9 | 116.99 |
C1—C6—C5 | 118.7 (4) | N1—C8—C9 | 126.12 |
C1—C6—C7 | 122.6 (3) | H10—C10—C11 | 119.77 |
C5—C6—C7 | 118.6 (3) | H10—C10—C9 | 119.74 |
N1—C7—C6 | 115.9 (3) | H12—C12—C13 | 118.96 |
N1—C7—C7i | 105.2 (2) | H12—C12—C11 | 118.94 |
C6—C7—C7i | 113.0 (2) | H15c—C15—H15b | 109.42 |
N1—C8—C9 | 126.2 (4) | H15c—C15—H15a | 109.39 |
C8—C9—C10 | 118.1 (5) | H15c—C15—C11 | 109.59 |
C8—C9—C14 | 119.9 (3) | H15b—C15—H15a | 109.43 |
C10—C9—C14 | 121.5 (4) | H15b—C15—C11 | 109.54 |
C11—C10—C9 | 120.5 (5) | H15a—C15—C11 | 109.46 |
C10—C11—C12 | 118.2 (4) | H16a—C16—H16b | 107.52 |
C10—C11—C15 | 120.8 (5) | H16a—C16—O2 | 108.63 |
C12—C11—C15 | 121.0 (4) | H16a—C16—C13 | 108.71 |
C13—C12—C11 | 122.1 (4) | H16b—C16—O2 | 108.68 |
C12—C13—C14 | 121.0 (4) | H16b—C16—C13 | 108.67 |
C12—C13—C16 | 121.5 (4) | H17a—C17—H17c | 109.49 |
C14—C13—C16 | 117.6 (4) | H17a—C17—H17b | 109.49 |
O1—C14—C13 | 119.5 (4) | H17a—C17—O2 | 109.52 |
O1—C14—C9 | 124.1 (4) | H17c—C17—H17b | 109.46 |
C13—C14—C9 | 116.4 (4) | H17c—C17—O2 | 109.44 |
O2—C16—C13 | 114.4 (4) | H17b—C17—O2 | 109.43 |
N2—Ni2—N2ii | 85.5 (2) | H18—C18—C19 | 119.57 |
N2—Ni2—O3 | 95.25 (11) | H18—C18—C23 | 119.57 |
N2ii—Ni2—O3 | 170.48 (15) | H19—C19—C20 | 119.35 |
N2—Ni2—O3ii | 170.48 (15) | H19—C19—C18 | 119.35 |
N2ii—Ni2—O3ii | 95.25 (11) | H20—C20—C21 | 120.58 |
O3—Ni2—O3ii | 85.58 (18) | H20—C20—C19 | 120.50 |
C31—O3—Ni2 | 125.9 (3) | H21—C21—C20 | 119.74 |
C33—O4—C34 | 112.3 (3) | H21—C21—C22 | 119.82 |
C25—N2—C24 | 119.3 (3) | H22—C22—C23 | 119.28 |
C25—N2—Ni2 | 126.1 (3) | H22—C22—C21 | 119.29 |
C24—N2—Ni2 | 114.0 (2) | H24—C24—N2 | 107.40 |
C19—C18—C23 | 120.8 (4) | H24—C24—C23 | 107.37 |
C20—C19—C18 | 121.4 (5) | H24—C24—C24 | 107.41 |
C21—C20—C19 | 118.9 (5) | H25—C25—N2 | 117.11 |
C20—C21—C22 | 120.4 (5) | H25—C25—C26 | 117.27 |
C23—C22—C21 | 121.4 (5) | H27—C27—C28 | 117.73 |
C22—C23—C18 | 117.1 (4) | H27—C27—C26 | 117.75 |
C22—C23—C24 | 121.8 (4) | H29—C29—C28 | 117.76 |
C18—C23—C24 | 121.1 (4) | H29—C29—C30 | 117.66 |
N2—C24—C23 | 116.1 (3) | H32a—C32—H32b | 109.45 |
N2—C24—C24ii | 105.1 (2) | H32a—C32—H32c | 109.47 |
C23—C24—C24ii | 113.1 (3) | H32a—C32—C28 | 109.49 |
N2—C25—C26 | 125.6 (4) | H32b—C32—H32c | 109.51 |
C27—C26—C31 | 118.5 (5) | H32b—C32—C28 | 109.42 |
C27—C26—C25 | 120.0 (5) | H32c—C32—C28 | 109.48 |
C31—C26—C25 | 121.3 (3) | H33a—C33—H33b | 107.56 |
C28—C27—C26 | 124.5 (5) | H33a—C33—O4 | 108.60 |
C27—C28—C29 | 115.7 (4) | H33a—C33—C30 | 108.65 |
C27—C28—C32 | 122.1 (4) | H33b—C33—O4 | 108.64 |
C29—C28—C32 | 122.2 (4) | H33b—C33—C30 | 108.65 |
C28—C29—C30 | 124.6 (4) | H34a—C34—H34b | 109.48 |
C29—C30—C31 | 118.4 (4) | H34a—C34—H34c | 109.44 |
C29—C30—C33 | 123.0 (4) | H34a—C34—O4 | 109.47 |
C31—C30—C33 | 118.6 (4) | H34b—C34—H34c | 109.45 |
O3—C31—C26 | 124.0 (4) | H34b—C34—O4 | 109.50 |
O3—C31—C30 | 117.7 (4) | H34c—C34—O4 | 109.49 |
C26—C31—C30 | 118.2 (4) | ||
O1i—Ni1—O1—C14 | −169.3 (4) | N2—Ni2—O3—C31 | 7.7 (3) |
N1—Ni1—O1—C14 | 7.8 (3) | N2ii—Ni2—O3—C31 | −86.4 (11) |
N1i—Ni1—O1—C14 | 111 (3) | O3ii—Ni2—O3—C31 | 178.1 (4) |
O1i—Ni1—N1—C8 | 65 (3) | N2ii—Ni2—N2—C25 | 175.5 (5) |
O1—Ni1—N1—C8 | −14.9 (3) | O3—Ni2—N2—C25 | 5.0 (4) |
N1i—Ni1—N1—C8 | 168.0 (4) | O3ii—Ni2—N2—C25 | −89.6 (11) |
O1i—Ni1—N1—C7 | −117 (3) | N2ii—Ni2—N2—C24 | −13.11 (17) |
O1—Ni1—N1—C7 | 163.6 (3) | O3—Ni2—N2—C24 | 176.4 (3) |
N1i—Ni1—N1—C7 | −13.56 (16) | O3ii—Ni2—N2—C24 | 81.8 (11) |
C6—C1—C2—C3 | 0.2 (6) | C23—C18—C19—C20 | −0.9 (8) |
C1—C2—C3—C4 | −2.1 (7) | C18—C19—C20—C21 | −0.5 (8) |
C2—C3—C4—C5 | 2.5 (8) | C19—C20—C21—C22 | 1.5 (9) |
C3—C4—C5—C6 | −1.0 (7) | C20—C21—C22—C23 | −1.2 (9) |
C2—C1—C6—C5 | 1.4 (5) | C21—C22—C23—C18 | −0.1 (7) |
C2—C1—C6—C7 | −176.7 (3) | C21—C22—C23—C24 | 177.0 (4) |
C4—C5—C6—C1 | −1.0 (6) | C19—C18—C23—C22 | 1.1 (6) |
C4—C5—C6—C7 | 177.1 (4) | C19—C18—C23—C24 | −176.0 (4) |
C8—N1—C7—C6 | −19.9 (5) | C25—N2—C24—C23 | −27.6 (5) |
Ni1—N1—C7—C6 | 161.6 (2) | Ni2—N2—C24—C23 | 160.3 (3) |
C8—N1—C7—C7i | −145.4 (4) | C25—N2—C24—C24ii | −153.3 (4) |
Ni1—N1—C7—C7i | 36.0 (4) | Ni2—N2—C24—C24ii | 34.6 (4) |
C1—C6—C7—N1 | −63.0 (4) | C22—C23—C24—N2 | 127.5 (4) |
C5—C6—C7—N1 | 118.9 (4) | C18—C23—C24—N2 | −55.6 (5) |
C1—C6—C7—C7i | 58.4 (5) | C22—C23—C24—C24ii | −111.0 (5) |
C5—C6—C7—C7i | −119.6 (4) | C18—C23—C24—C24ii | 66.0 (5) |
C7—N1—C8—C9 | −168.5 (3) | C24—N2—C25—C26 | 178.5 (3) |
Ni1—N1—C8—C9 | 9.9 (6) | Ni2—N2—C25—C26 | −10.5 (6) |
N1—C8—C9—C10 | 178.5 (4) | N2—C25—C26—C27 | −172.0 (4) |
N1—C8—C9—C14 | 6.3 (6) | N2—C25—C26—C31 | 3.3 (6) |
C8—C9—C10—C11 | −170.1 (4) | C31—C26—C27—C28 | −2.4 (6) |
C14—C9—C10—C11 | 2.0 (6) | C25—C26—C27—C28 | 173.0 (4) |
C9—C10—C11—C12 | 2.9 (6) | C26—C27—C28—C29 | 0.4 (6) |
C9—C10—C11—C15 | −178.7 (4) | C26—C27—C28—C32 | 178.6 (4) |
C10—C11—C12—C13 | −4.1 (7) | C27—C28—C29—C30 | 0.0 (7) |
C15—C11—C12—C13 | 177.5 (4) | C32—C28—C29—C30 | −178.2 (4) |
C11—C12—C13—C14 | 0.3 (6) | C28—C29—C30—C31 | 1.6 (6) |
C11—C12—C13—C16 | 179.5 (4) | C28—C29—C30—C33 | −178.8 (4) |
Ni1—O1—C14—C13 | −175.8 (3) | Ni2—O3—C31—C26 | −15.7 (6) |
Ni1—O1—C14—C9 | 4.4 (6) | Ni2—O3—C31—C30 | 166.2 (3) |
C12—C13—C14—O1 | −175.4 (4) | C27—C26—C31—O3 | −174.1 (3) |
C16—C13—C14—O1 | 5.4 (6) | C25—C26—C31—O3 | 10.5 (6) |
C12—C13—C14—C9 | 4.4 (6) | C27—C26—C31—C30 | 3.9 (5) |
C16—C13—C14—C9 | −174.8 (3) | C25—C26—C31—C30 | −171.5 (3) |
C8—C9—C14—O1 | −13.8 (5) | C29—C30—C31—O3 | 174.6 (3) |
C10—C9—C14—O1 | 174.3 (3) | C33—C30—C31—O3 | −4.9 (6) |
C8—C9—C14—C13 | 166.3 (4) | C29—C30—C31—C26 | −3.6 (6) |
C10—C9—C14—C13 | −5.6 (5) | C33—C30—C31—C26 | 176.9 (3) |
C17—O2—C16—C13 | −80.6 (5) | C34—O4—C33—C30 | 80.5 (5) |
C12—C13—C16—O2 | −21.3 (6) | C29—C30—C33—O4 | 18.4 (6) |
C14—C13—C16—O2 | 158.0 (4) | C31—C30—C33—O4 | −162.1 (4) |
Symmetry codes: (i) −x+1, y, −z; (ii) −x+1, y, −z+1. |
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