Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804029952/ac6127sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804029952/ac6127Isup2.hkl |
CCDC reference: 259079
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- Disorder in solvent or counterion
- R factor = 0.074
- wR factor = 0.200
- Data-to-parameter ratio = 11.8
checkCIF/PLATON results
No syntax errors found
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.743 0.902 Tmin' and Tmax expected: 0.876 0.902 RR' = 0.848 Please check that your absorption correction is appropriate. PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.85 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT214_ALERT_2_C Atom C14 (Anion/Solvent) ADP max/min Ratio 4.80 prolat PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for N2 PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors for C11' PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for N3 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for N4 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors for B1 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 29.00 Perc. PLAT309_ALERT_2_C Single Bonded Oxygen (C-O .GT. 1.3 Ang) ........ O3 PLAT309_ALERT_2_C Single Bonded Oxygen (C-O .GT. 1.3 Ang) ........ O3' PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9 PLAT380_ALERT_4_C Incorrectly Oriented X(sp2)-Methyl Moiety ...... C10 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 1 O1 -NI1 -O1 -C6 109.00100.00 2.577 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 8 N1 -NI1 -N1 -C1 -152.00100.00 2.577 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 13 N1 -NI1 -N1 -C5 30.00100.00 2.577 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 39 O3 -C11 -N3 -C12' -125.00 8.00 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 45 O3' -C11'-N3 -C13 163.00 21.00 1.555 1.555 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.433(18), Rep 1.432(8) ...... 2.25 su-Rat C16 -N4 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 40.70 Deg. F4' -B1 -F3 1.555 1.555 1.555 PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 31.60 Deg. F3' -B1 -F4 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 23 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 12 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
[Ni(C10H12N2O)2(H2O)2](BF4)2·4C3H7NO | Z = 1 |
Mr = 913.18 | F(000) = 478 |
Triclinic, P1 | Dx = 1.343 Mg m−3 |
a = 10.036 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 10.384 (3) Å | Cell parameters from 652 reflections |
c = 13.384 (3) Å | θ = 3.2–23.0° |
α = 107.744 (5)° | µ = 0.52 mm−1 |
β = 93.331 (5)° | T = 293 K |
γ = 118.732 (5)° | Block, green |
V = 1129.4 (5) Å3 | 0.25 × 0.22 × 0.20 mm |
Bruker SMART CCD area-detector diffractometer | 3835 independent reflections |
Radiation source: fine-focus sealed tube | 2265 reflections with I > 2s/(I) |
Graphite monochromator | Rint = 0.040 |
φ and ω scans | θmax = 25.1°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.743, Tmax = 0.902 | k = −12→12 |
5657 measured reflections | l = −14→15 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.074 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.201 | H atoms treated by a mixture of independent and constrained refinement |
S = 0.98 | w = 1/[σ2(Fo2) + (0.1115P)2] where P = (Fo2 + 2Fc2)/3 |
3835 reflections | (Δ/σ)max < 0.001 |
324 parameters | Δρmax = 0.84 e Å−3 |
37 restraints | Δρmin = −0.54 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. |
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 | Occ. (<1) | |
Ni1 | 0.0000 | 1.0000 | 1.0000 | 0.0422 (4) | |
O1 | 0.0636 (5) | 0.8447 (4) | 1.0085 (3) | 0.0470 (10) | |
N1 | 0.0135 (5) | 0.9157 (5) | 0.8445 (3) | 0.0418 (11) | |
N2 | 0.2342 (6) | 0.5608 (5) | 1.0142 (4) | 0.0536 (13) | |
C1 | −0.0127 (7) | 0.9592 (7) | 0.7651 (5) | 0.0509 (15) | |
H1A | −0.0359 | 1.0387 | 0.7803 | 0.061* | |
C2 | −0.0064 (8) | 0.8910 (8) | 0.6625 (5) | 0.0597 (17) | |
H2A | −0.0225 | 0.9257 | 0.6091 | 0.072* | |
C3 | 0.0239 (8) | 0.7699 (8) | 0.6381 (5) | 0.0635 (18) | |
H3A | 0.0255 | 0.7195 | 0.5681 | 0.076* | |
C4 | 0.0516 (7) | 0.7259 (7) | 0.7208 (5) | 0.0540 (16) | |
H4A | 0.0724 | 0.6448 | 0.7068 | 0.065* | |
C5 | 0.0486 (6) | 0.8020 (6) | 0.8239 (4) | 0.0409 (13) | |
C6 | 0.0846 (6) | 0.7735 (6) | 0.9222 (4) | 0.0398 (13) | |
C7 | 0.1389 (7) | 0.6697 (7) | 0.9149 (5) | 0.0478 (14) | |
H7A | 0.1487 | 0.6161 | 0.8488 | 0.057* | |
C8 | 0.1774 (7) | 0.6481 (7) | 1.0060 (5) | 0.0491 (15) | |
H8A | 0.1613 | 0.7016 | 1.0691 | 0.059* | |
C9 | 0.2788 (8) | 0.5558 (8) | 1.1166 (6) | 0.069 (2) | |
H9A | 0.2542 | 0.6191 | 1.1720 | 0.104* | |
H9B | 0.3894 | 0.5970 | 1.1341 | 0.104* | |
H9C | 0.2225 | 0.4481 | 1.1121 | 0.104* | |
C10 | 0.2652 (11) | 0.4710 (10) | 0.9198 (6) | 0.092 (3) | |
H10A | 0.2308 | 0.4827 | 0.8565 | 0.138* | |
H10B | 0.2095 | 0.3607 | 0.9095 | 0.138* | |
H10C | 0.3756 | 0.5109 | 0.9320 | 0.138* | |
C11 | 0.6093 (13) | 0.5298 (16) | 0.6777 (10) | 0.106 (7) | 0.64 (2) |
H11A | 0.7102 | 0.5617 | 0.6688 | 0.127* | 0.64 (2) |
C12 | 0.3201 (13) | 0.359 (2) | 0.6150 (14) | 0.165 (11) | 0.64 (2) |
H12A | 0.2616 | 0.2608 | 0.6251 | 0.247* | 0.64 (2) |
H12B | 0.2661 | 0.3526 | 0.5504 | 0.247* | 0.64 (2) |
H12C | 0.3304 | 0.4442 | 0.6760 | 0.247* | 0.64 (2) |
C13 | 0.487 (3) | 0.285 (2) | 0.5112 (11) | 0.141 (10) | 0.64 (2) |
H13A | 0.3840 | 0.1958 | 0.4710 | 0.211* | 0.64 (2) |
H13B | 0.5493 | 0.2471 | 0.5338 | 0.211* | 0.64 (2) |
H13C | 0.5352 | 0.3416 | 0.4663 | 0.211* | 0.64 (2) |
O3 | 0.5784 (15) | 0.6128 (15) | 0.7602 (10) | 0.108 (6) | 0.64 (2) |
O3' | 0.600 (4) | 0.598 (5) | 0.736 (3) | 0.18 (2) | 0.36 (2) |
C11' | 0.449 (4) | 0.481 (4) | 0.698 (2) | 0.18 (3) | 0.36 (2) |
H11B | 0.3600 | 0.4650 | 0.7224 | 0.219* | 0.36 (2) |
C12' | 0.350 (3) | 0.232 (2) | 0.5342 (19) | 0.16 (2) | 0.36 (2) |
H12D | 0.2517 | 0.2143 | 0.5503 | 0.242* | 0.36 (2) |
H12E | 0.3687 | 0.1542 | 0.5445 | 0.242* | 0.36 (2) |
H12F | 0.3454 | 0.2231 | 0.4604 | 0.242* | 0.36 (2) |
C13' | 0.633 (2) | 0.435 (4) | 0.594 (4) | 0.19 (2) | 0.36 (2) |
H13D | 0.6541 | 0.3560 | 0.5993 | 0.286* | 0.36 (2) |
H13E | 0.7060 | 0.5353 | 0.6512 | 0.286* | 0.36 (2) |
H13F | 0.6425 | 0.4438 | 0.5255 | 0.286* | 0.36 (2) |
C14 | 0.4328 (11) | 1.0661 (11) | 0.8836 (9) | 0.159 (7) | |
H14A | 0.4441 | 1.0345 | 0.9424 | 0.191* | |
C15 | 0.4395 (12) | 1.0159 (14) | 0.6821 (7) | 0.126 (4) | |
H15A | 0.4785 | 0.9658 | 0.6296 | 0.190* | |
H15B | 0.3284 | 0.9658 | 0.6562 | 0.190* | |
H15C | 0.4900 | 1.1264 | 0.6934 | 0.190* | |
C16 | 0.5486 (15) | 0.9215 (14) | 0.7940 (9) | 0.147 (4) | |
H16A | 0.5726 | 0.8845 | 0.7266 | 0.220* | |
H16B | 0.6437 | 0.9907 | 0.8503 | 0.220* | |
H16C | 0.4797 | 0.8324 | 0.8113 | 0.220* | |
B1 | 0.1042 (10) | 0.7621 (10) | 0.3590 (6) | 0.075 (2) | |
F1 | 0.1212 (8) | 0.7738 (8) | 0.2633 (4) | 0.145 (2) | |
F2 | −0.0272 (10) | 0.6284 (8) | 0.3498 (6) | 0.171 (3) | |
F3 | 0.2379 (17) | 0.805 (4) | 0.4221 (16) | 0.168 (12) | 0.52 (4) |
F4 | 0.049 (4) | 0.855 (4) | 0.406 (2) | 0.200 (13) | 0.52 (4) |
F3' | 0.131 (3) | 0.8928 (15) | 0.4327 (12) | 0.158 (11) | 0.48 (4) |
F4' | 0.179 (3) | 0.696 (3) | 0.3867 (18) | 0.176 (10) | 0.48 (4) |
N3 | 0.4744 (8) | 0.3885 (8) | 0.6050 (5) | 0.0828 (19) | |
N4 | 0.4718 (8) | 1.0044 (8) | 0.7837 (5) | 0.0818 (19) | |
O2 | 0.2371 (5) | 1.1800 (5) | 1.0426 (3) | 0.0574 (11) | |
H2B | 0.2900 | 1.1860 | 0.9950 | 0.069* | |
H2C | 0.2803 | 1.2471 | 1.1073 | 0.069* | |
O4 | 0.3877 (12) | 1.1488 (12) | 0.8901 (9) | 0.229 (7) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0527 (8) | 0.0454 (7) | 0.0353 (6) | 0.0324 (6) | 0.0096 (5) | 0.0126 (5) |
O1 | 0.068 (3) | 0.053 (2) | 0.033 (2) | 0.045 (2) | 0.0110 (18) | 0.0110 (18) |
N1 | 0.047 (3) | 0.042 (3) | 0.037 (3) | 0.026 (2) | 0.007 (2) | 0.013 (2) |
N2 | 0.057 (3) | 0.046 (3) | 0.065 (3) | 0.033 (3) | 0.009 (3) | 0.022 (3) |
C1 | 0.058 (4) | 0.057 (4) | 0.044 (4) | 0.033 (3) | 0.010 (3) | 0.022 (3) |
C2 | 0.074 (5) | 0.067 (4) | 0.038 (4) | 0.037 (4) | 0.005 (3) | 0.021 (3) |
C3 | 0.071 (5) | 0.073 (5) | 0.036 (3) | 0.034 (4) | 0.013 (3) | 0.015 (3) |
C4 | 0.061 (4) | 0.058 (4) | 0.045 (4) | 0.036 (3) | 0.016 (3) | 0.012 (3) |
C5 | 0.040 (3) | 0.039 (3) | 0.040 (3) | 0.022 (3) | 0.010 (2) | 0.008 (2) |
C6 | 0.037 (3) | 0.035 (3) | 0.047 (3) | 0.018 (3) | 0.009 (2) | 0.016 (3) |
C7 | 0.051 (4) | 0.047 (3) | 0.051 (4) | 0.032 (3) | 0.013 (3) | 0.014 (3) |
C8 | 0.048 (4) | 0.042 (3) | 0.059 (4) | 0.028 (3) | 0.011 (3) | 0.013 (3) |
C9 | 0.062 (5) | 0.060 (4) | 0.086 (5) | 0.031 (4) | 0.002 (4) | 0.033 (4) |
C10 | 0.119 (7) | 0.111 (6) | 0.102 (6) | 0.100 (6) | 0.033 (5) | 0.042 (5) |
C11 | 0.108 (14) | 0.19 (2) | 0.098 (14) | 0.116 (16) | 0.050 (12) | 0.086 (15) |
C12 | 0.058 (11) | 0.18 (2) | 0.107 (15) | 0.016 (11) | −0.009 (9) | −0.034 (13) |
C13 | 0.22 (3) | 0.17 (2) | 0.075 (11) | 0.14 (2) | 0.061 (14) | 0.025 (12) |
O3 | 0.125 (11) | 0.080 (8) | 0.056 (7) | 0.056 (7) | −0.037 (7) | −0.042 (6) |
O3' | 0.25 (4) | 0.34 (6) | 0.19 (4) | 0.25 (4) | 0.16 (3) | 0.20 (4) |
C11' | 0.26 (7) | 0.23 (6) | 0.11 (3) | 0.17 (6) | 0.02 (4) | 0.06 (4) |
C12' | 0.18 (4) | 0.14 (3) | 0.053 (18) | 0.01 (3) | 0.01 (2) | 0.016 (18) |
C13' | 0.09 (3) | 0.17 (4) | 0.27 (6) | 0.05 (3) | 0.06 (3) | 0.06 (4) |
C14 | 0.032 (5) | 0.043 (5) | 0.32 (2) | −0.012 (4) | 0.007 (8) | 0.028 (9) |
C15 | 0.112 (8) | 0.181 (11) | 0.090 (7) | 0.072 (8) | 0.026 (6) | 0.063 (7) |
C16 | 0.168 (12) | 0.170 (11) | 0.151 (10) | 0.132 (11) | 0.024 (8) | 0.051 (8) |
B1 | 0.086 (7) | 0.086 (7) | 0.063 (6) | 0.047 (6) | 0.028 (5) | 0.036 (5) |
F1 | 0.211 (7) | 0.207 (6) | 0.083 (4) | 0.139 (6) | 0.067 (4) | 0.078 (4) |
F2 | 0.203 (8) | 0.105 (5) | 0.157 (6) | 0.054 (5) | 0.077 (6) | 0.032 (4) |
F3 | 0.131 (13) | 0.26 (3) | 0.121 (14) | 0.101 (17) | 0.002 (9) | 0.085 (17) |
F4 | 0.33 (3) | 0.26 (3) | 0.21 (2) | 0.24 (3) | 0.20 (2) | 0.158 (19) |
F3' | 0.29 (3) | 0.035 (7) | 0.067 (9) | 0.050 (11) | 0.011 (13) | −0.010 (6) |
F4' | 0.19 (2) | 0.133 (17) | 0.21 (2) | 0.109 (17) | −0.019 (15) | 0.049 (14) |
N3 | 0.085 (5) | 0.088 (5) | 0.058 (4) | 0.043 (4) | −0.004 (4) | 0.013 (4) |
N4 | 0.085 (5) | 0.084 (5) | 0.071 (4) | 0.047 (4) | 0.023 (3) | 0.017 (4) |
O2 | 0.056 (3) | 0.053 (2) | 0.048 (2) | 0.026 (2) | 0.0070 (19) | 0.006 (2) |
O4 | 0.132 (9) | 0.157 (9) | 0.238 (12) | 0.006 (7) | 0.099 (8) | −0.013 (8) |
Ni1—O1 | 2.028 (3) | C12—H12B | 0.9600 |
Ni1—O1i | 2.028 (3) | C12—H12C | 0.9600 |
Ni1—N1 | 2.038 (4) | C13—N3 | 1.441 (9) |
Ni1—N1i | 2.038 (4) | C13—H13A | 0.9600 |
Ni1—O2i | 2.097 (4) | C13—H13B | 0.9600 |
Ni1—O2 | 2.097 (4) | C13—H13C | 0.9600 |
O1—C6 | 1.259 (6) | O3'—C11' | 1.339 (9) |
N1—C1 | 1.333 (7) | C11'—N3 | 1.439 (11) |
N1—C5 | 1.344 (7) | C11'—H11B | 0.9300 |
N2—C8 | 1.307 (7) | C12'—N3 | 1.440 (10) |
N2—C9 | 1.441 (8) | C12'—H12D | 0.9600 |
N2—C10 | 1.472 (8) | C12'—H12E | 0.9600 |
C1—C2 | 1.360 (8) | C12'—H12F | 0.9600 |
C1—H1A | 0.9300 | C13'—N3 | 1.452 (11) |
C2—C3 | 1.382 (9) | C13'—H13D | 0.9600 |
C2—H2A | 0.9300 | C13'—H13E | 0.9600 |
C3—C4 | 1.380 (9) | C13'—H13F | 0.9600 |
C3—H3A | 0.9300 | C14—O4 | 1.134 (10) |
C4—C5 | 1.376 (7) | C14—N4 | 1.460 (9) |
C4—H4A | 0.9300 | C14—H14A | 0.9599 |
C5—C6 | 1.494 (8) | C15—N4 | 1.433 (7) |
C6—C7 | 1.406 (7) | C15—H15A | 0.9600 |
C7—C8 | 1.371 (8) | C15—H15B | 0.9600 |
C7—H7A | 0.9300 | C15—H15C | 0.9600 |
C8—H8A | 0.9300 | C16—N4 | 1.432 (8) |
C9—H9A | 0.9600 | C16—H16A | 0.9600 |
C9—H9B | 0.9600 | C16—H16B | 0.9600 |
C9—H9C | 0.9600 | C16—H16C | 0.9600 |
C10—H10A | 0.9600 | B1—F3' | 1.300 (9) |
C10—H10B | 0.9600 | B1—F4' | 1.335 (10) |
C10—H10C | 0.9600 | B1—F3 | 1.331 (9) |
C11—O3 | 1.332 (8) | B1—F1 | 1.336 (7) |
C11—N3 | 1.414 (10) | B1—F4 | 1.345 (10) |
C11—H11A | 0.9300 | B1—F2 | 1.342 (8) |
C12—N3 | 1.450 (9) | O2—H2B | 0.8501 |
C12—H12A | 0.9600 | O2—H2C | 0.8500 |
O1—Ni1—O1i | 180.000 (3) | N3—C13—H13C | 109.5 |
O1—Ni1—N1 | 80.00 (16) | H13A—C13—H13C | 109.5 |
O1i—Ni1—N1 | 100.00 (16) | H13B—C13—H13C | 109.5 |
O1—Ni1—N1i | 100.00 (16) | O3'—C11'—N3 | 95 (3) |
O1i—Ni1—N1i | 80.00 (16) | O3'—C11'—H11B | 132.6 |
N1—Ni1—N1i | 180.000 (2) | N3—C11'—H11B | 132.6 |
O1—Ni1—O2i | 90.27 (16) | N3—C12'—H12D | 109.5 |
O1i—Ni1—O2i | 89.73 (16) | N3—C12'—H12E | 109.5 |
N1—Ni1—O2i | 90.02 (17) | H12D—C12'—H12E | 109.5 |
N1i—Ni1—O2i | 89.98 (17) | N3—C12'—H12F | 109.5 |
O1—Ni1—O2 | 89.73 (16) | H12D—C12'—H12F | 109.5 |
O1i—Ni1—O2 | 90.27 (16) | H12E—C12'—H12F | 109.5 |
N1—Ni1—O2 | 89.98 (17) | N3—C13'—H13D | 109.5 |
N1i—Ni1—O2 | 90.02 (17) | N3—C13'—H13E | 109.5 |
O2i—Ni1—O2 | 180.0 | H13D—C13'—H13E | 109.5 |
C6—O1—Ni1 | 115.1 (3) | N3—C13'—H13F | 109.5 |
C1—N1—C5 | 119.6 (5) | H13D—C13'—H13F | 109.5 |
C1—N1—Ni1 | 126.6 (4) | H13E—C13'—H13F | 109.5 |
C5—N1—Ni1 | 113.7 (3) | O4—C14—N4 | 119.5 (12) |
C8—N2—C9 | 121.8 (5) | O4—C14—H14A | 120.9 |
C8—N2—C10 | 121.2 (5) | N4—C14—H14A | 119.6 |
C9—N2—C10 | 116.8 (5) | N4—C15—H15A | 110.9 |
N1—C1—C2 | 122.0 (6) | N4—C15—H15B | 109.3 |
N1—C1—H1A | 119.0 | H15A—C15—H15B | 109.5 |
C2—C1—H1A | 119.0 | N4—C15—H15C | 108.2 |
C1—C2—C3 | 119.6 (6) | H15A—C15—H15C | 109.5 |
C1—C2—H2A | 120.2 | H15B—C15—H15C | 109.5 |
C3—C2—H2A | 120.2 | N4—C16—H16A | 109.2 |
C2—C3—C4 | 118.1 (6) | N4—C16—H16B | 110.2 |
C2—C3—H3A | 120.9 | H16A—C16—H16B | 109.5 |
C4—C3—H3A | 120.9 | N4—C16—H16C | 109.0 |
C5—C4—C3 | 120.0 (6) | H16A—C16—H16C | 109.5 |
C5—C4—H4A | 120.0 | H16B—C16—H16C | 109.5 |
C3—C4—H4A | 120.0 | F3'—B1—F4' | 116.0 (12) |
N1—C5—C4 | 120.6 (5) | F3'—B1—F3 | 80.2 (15) |
N1—C5—C6 | 113.4 (4) | F4'—B1—F3 | 40.7 (11) |
C4—C5—C6 | 126.0 (5) | F3'—B1—F1 | 113.0 (10) |
O1—C6—C7 | 123.0 (5) | F4'—B1—F1 | 111.3 (12) |
O1—C6—C5 | 117.4 (4) | F3—B1—F1 | 112.4 (9) |
C7—C6—C5 | 119.6 (5) | F3'—B1—F4 | 31.6 (17) |
C8—C7—C6 | 119.6 (5) | F4'—B1—F4 | 139.2 (15) |
C8—C7—H7A | 120.2 | F3—B1—F4 | 110.6 (13) |
C6—C7—H7A | 120.2 | F1—B1—F4 | 107.0 (10) |
N2—C8—C7 | 127.4 (6) | F3'—B1—F2 | 116.3 (12) |
N2—C8—H8A | 116.3 | F4'—B1—F2 | 85.1 (14) |
C7—C8—H8A | 116.3 | F3—B1—F2 | 119.1 (14) |
N2—C9—H9A | 109.5 | F1—B1—F2 | 112.3 (7) |
N2—C9—H9B | 109.5 | F4—B1—F2 | 93.2 (16) |
H9A—C9—H9B | 109.5 | C11—N3—C11' | 63.5 (15) |
N2—C9—H9C | 109.5 | C11—N3—C12' | 170.7 (17) |
H9A—C9—H9C | 109.5 | C11'—N3—C12' | 121.2 (15) |
H9B—C9—H9C | 109.5 | C11—N3—C13 | 121.0 (11) |
N2—C10—H10A | 109.5 | C11'—N3—C13 | 175.2 (16) |
N2—C10—H10B | 109.5 | C12'—N3—C13 | 54.1 (12) |
H10A—C10—H10B | 109.5 | C11—N3—C12 | 119.7 (8) |
N2—C10—H10C | 109.5 | C11'—N3—C12 | 57.2 (14) |
H10A—C10—H10C | 109.5 | C12'—N3—C12 | 67.0 (15) |
H10B—C10—H10C | 109.5 | C13—N3—C12 | 118.6 (10) |
O3—C11—N3 | 113.7 (10) | C11—N3—C13' | 56.7 (14) |
O3—C11—H11A | 123.1 | C11'—N3—C13' | 120.1 (15) |
N3—C11—H11A | 123.1 | C12'—N3—C13' | 117.3 (14) |
N3—C12—H12A | 109.5 | C13—N3—C13' | 64.3 (14) |
N3—C12—H12B | 109.5 | C12—N3—C13' | 174 (2) |
H12A—C12—H12B | 109.5 | C16—N4—C15 | 119.7 (7) |
N3—C12—H12C | 109.5 | C16—N4—C14 | 112.5 (7) |
H12A—C12—H12C | 109.5 | C15—N4—C14 | 127.8 (7) |
H12B—C12—H12C | 109.5 | Ni1—O2—H2B | 120.0 |
N3—C13—H13A | 109.5 | Ni1—O2—H2C | 120.0 |
N3—C13—H13B | 109.5 | H2B—O2—H2C | 120.0 |
H13A—C13—H13B | 109.5 | ||
O1i—Ni1—O1—C6 | 109 (100) | C3—C4—C5—C6 | −176.5 (6) |
N1—Ni1—O1—C6 | 1.3 (4) | Ni1—O1—C6—C7 | 175.7 (4) |
N1i—Ni1—O1—C6 | −178.7 (4) | Ni1—O1—C6—C5 | −4.6 (6) |
O2i—Ni1—O1—C6 | 91.2 (4) | N1—C5—C6—O1 | 6.8 (7) |
O2—Ni1—O1—C6 | −88.8 (4) | C4—C5—C6—O1 | −174.4 (5) |
O1—Ni1—N1—C1 | −179.3 (5) | N1—C5—C6—C7 | −173.5 (5) |
O1i—Ni1—N1—C1 | 0.7 (5) | C4—C5—C6—C7 | 5.4 (9) |
N1i—Ni1—N1—C1 | −152 (100) | O1—C6—C7—C8 | −2.7 (9) |
O2i—Ni1—N1—C1 | 90.4 (5) | C5—C6—C7—C8 | 177.6 (5) |
O2—Ni1—N1—C1 | −89.6 (5) | C9—N2—C8—C7 | 176.1 (6) |
O1—Ni1—N1—C5 | 2.6 (4) | C10—N2—C8—C7 | 0.2 (10) |
O1i—Ni1—N1—C5 | −177.4 (4) | C6—C7—C8—N2 | −177.6 (6) |
N1i—Ni1—N1—C5 | 30 (100) | O3—C11—N3—C11' | −2 (2) |
O2i—Ni1—N1—C5 | −87.7 (4) | O3—C11—N3—C12' | −125 (8) |
O2—Ni1—N1—C5 | 92.3 (4) | O3—C11—N3—C13 | 179.9 (15) |
C5—N1—C1—C2 | 0.6 (9) | O3—C11—N3—C12 | 9 (2) |
Ni1—N1—C1—C2 | −177.4 (5) | O3—C11—N3—C13' | −177 (3) |
N1—C1—C2—C3 | 1.7 (10) | O3'—C11'—N3—C11 | 3 (3) |
C1—C2—C3—C4 | −2.0 (10) | O3'—C11'—N3—C12' | 174 (3) |
C2—C3—C4—C5 | 0.0 (10) | O3'—C11'—N3—C13 | 163 (21) |
C1—N1—C5—C4 | −2.6 (8) | O3'—C11'—N3—C12 | −165 (5) |
Ni1—N1—C5—C4 | 175.7 (4) | O3'—C11'—N3—C13' | 8 (5) |
C1—N1—C5—C6 | 176.4 (5) | O4—C14—N4—C16 | 171.3 (11) |
Ni1—N1—C5—C6 | −5.4 (6) | O4—C14—N4—C15 | −9.9 (16) |
C3—C4—C5—N1 | 2.3 (9) |
Symmetry code: (i) −x, −y+2, −z+2. |