Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806024330/ww2017sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806024330/ww2017Isup2.hkl |
CCDC reference: 613848
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.015 Å
- Disorder in solvent or counterion
- R factor = 0.064
- wR factor = 0.131
- Data-to-parameter ratio = 11.4
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT026_ALERT_3_B Ratio Observed / Unique Reflections too Low .... 34 Perc.
Alert level C RINTA01_ALERT_3_C The value of Rint is greater than 0.10 Rint given 0.120 PLAT020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.12 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Ni1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl2 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 41.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 15 PLAT480_ALERT_4_C Long H...A H-Bond Reported H2 .. CL1 .. 2.95 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H4B .. O6' .. 2.64 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H4B .. O5 .. 2.66 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H5B .. CL2 .. 2.94 Ang.
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 7 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); 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(C11H29N5)](ClO4)2 | F(000) = 1024 |
Mr = 489.00 | Dx = 1.627 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 882 reflections |
a = 9.454 (4) Å | θ = 2.6–15.9° |
b = 14.589 (7) Å | µ = 1.29 mm−1 |
c = 14.477 (7) Å | T = 298 K |
β = 90.285 (8)° | Block, blue–purple |
V = 1996.6 (16) Å3 | 0.42 × 0.30 × 0.19 mm |
Z = 4 |
Bruker SMART CCD area-detector diffractometer | 3526 independent reflections |
Radiation source: fine-focus sealed tube | 1216 reflections with I > σ(I) |
Graphite monochromator | Rint = 0.120 |
φ and ω scans | θmax = 25.0°, θmin = 2.0° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −11→11 |
Tmin = 0.614, Tmax = 0.792 | k = −17→11 |
10278 measured reflections | l = −17→16 |
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)] = 0.064 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.131 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0268P)2] where P = (Fo2 + 2Fc2)/3 |
3526 reflections | (Δ/σ)max < 0.001 |
309 parameters | Δρmax = 0.48 e Å−3 |
655 restraints | Δρmin = −0.41 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. |
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 > 2σ(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 | 0.27513 (10) | 0.22865 (7) | 0.41737 (7) | 0.0534 (4) | |
Cl1 | 0.2966 (3) | 0.20870 (19) | 0.12416 (17) | 0.0691 (7) | |
Cl2 | 0.3749 (3) | 0.0277 (2) | 0.65403 (19) | 0.0765 (8) | |
N1 | 0.2535 (7) | 0.0906 (4) | 0.3952 (5) | 0.085 (2) | |
H1A | 0.2965 | 0.0776 | 0.3414 | 0.102* | |
H1B | 0.3023 | 0.0616 | 0.4400 | 0.102* | |
N2 | 0.0920 (7) | 0.2547 (5) | 0.3447 (5) | 0.078 (2) | |
H2 | 0.1191 | 0.2547 | 0.2844 | 0.093* | |
N3 | 0.3067 (8) | 0.3694 (5) | 0.4042 (5) | 0.073 (2) | |
N4 | 0.4817 (6) | 0.2105 (4) | 0.4505 (4) | 0.069 (2) | |
H4A | 0.4992 | 0.2378 | 0.5051 | 0.083* | |
H4B | 0.4984 | 0.1502 | 0.4574 | 0.083* | |
N5 | 0.1922 (6) | 0.2329 (4) | 0.5452 (4) | 0.070 (2) | |
H5A | 0.0976 | 0.2370 | 0.5388 | 0.083* | |
H5B | 0.2104 | 0.1786 | 0.5723 | 0.083* | |
O1 | 0.153 (2) | 0.178 (2) | 0.1141 (18) | 0.092 (6) | 0.44 (4) |
O2 | 0.302 (4) | 0.2993 (17) | 0.106 (2) | 0.130 (7) | 0.44 (4) |
O3 | 0.377 (3) | 0.165 (2) | 0.0593 (17) | 0.112 (7) | 0.44 (4) |
O1' | 0.368 (2) | 0.2862 (13) | 0.0877 (13) | 0.108 (5) | 0.56 (4) |
O2' | 0.327 (3) | 0.1328 (12) | 0.0672 (13) | 0.114 (6) | 0.56 (4) |
O3' | 0.1498 (13) | 0.225 (2) | 0.1266 (12) | 0.094 (5) | 0.56 (4) |
O4 | 0.3413 (6) | 0.1918 (5) | 0.2145 (4) | 0.118 (2) | |
O5 | 0.4709 (13) | 0.0972 (10) | 0.6320 (8) | 0.142 (4) | 0.743 (9) |
O6 | 0.4428 (14) | −0.0327 (7) | 0.7138 (8) | 0.131 (4) | 0.743 (9) |
O7 | 0.3495 (14) | −0.0190 (8) | 0.5722 (7) | 0.141 (4) | 0.743 (9) |
O8 | 0.2616 (11) | 0.0655 (8) | 0.6948 (8) | 0.133 (4) | 0.743 (9) |
O5' | 0.269 (2) | 0.0154 (19) | 0.5840 (16) | 0.110 (7) | 0.257 (9) |
O6' | 0.5088 (18) | 0.011 (2) | 0.626 (2) | 0.141 (8) | 0.257 (9) |
O7' | 0.334 (3) | −0.019 (2) | 0.7331 (14) | 0.113 (7) | 0.257 (9) |
O8' | 0.366 (4) | 0.1261 (11) | 0.6757 (18) | 0.115 (7) | 0.257 (9) |
C1 | 0.1111 (11) | 0.0493 (6) | 0.3915 (7) | 0.098 (3) | |
H1C | 0.1196 | −0.0145 | 0.3735 | 0.118* | |
H1D | 0.0701 | 0.0510 | 0.4527 | 0.118* | |
C2 | 0.0148 (10) | 0.0960 (8) | 0.3265 (7) | 0.111 (3) | |
H2A | 0.0577 | 0.0947 | 0.2658 | 0.133* | |
H2B | −0.0721 | 0.0607 | 0.3228 | 0.133* | |
C3 | −0.0223 (10) | 0.1914 (7) | 0.3479 (7) | 0.100 (3) | |
H3A | −0.0946 | 0.2114 | 0.3047 | 0.120* | |
H3B | −0.0630 | 0.1933 | 0.4093 | 0.120* | |
C4 | 0.0569 (9) | 0.3514 (7) | 0.3643 (6) | 0.092 (3) | |
H4C | −0.0144 | 0.3727 | 0.3209 | 0.111* | |
H4D | 0.0189 | 0.3567 | 0.4261 | 0.111* | |
C5 | 0.1822 (11) | 0.4069 (7) | 0.3563 (6) | 0.097 (3) | |
H5C | 0.1623 | 0.4673 | 0.3810 | 0.116* | |
H5D | 0.2044 | 0.4140 | 0.2914 | 0.116* | |
C6 | 0.4351 (13) | 0.3893 (6) | 0.3442 (6) | 0.096 (4) | |
H6A | 0.4159 | 0.3669 | 0.2823 | 0.115* | |
H6B | 0.4469 | 0.4553 | 0.3402 | 0.115* | |
C7 | 0.5715 (11) | 0.3482 (9) | 0.3773 (7) | 0.107 (4) | |
H7A | 0.6464 | 0.3695 | 0.3371 | 0.128* | |
H7B | 0.5912 | 0.3721 | 0.4386 | 0.128* | |
C8 | 0.5794 (10) | 0.2472 (7) | 0.3818 (6) | 0.089 (3) | |
H8A | 0.5565 | 0.2218 | 0.3216 | 0.107* | |
H8B | 0.6752 | 0.2289 | 0.3974 | 0.107* | |
C9 | 0.3289 (10) | 0.4193 (6) | 0.4932 (7) | 0.089 (3) | |
H9A | 0.3255 | 0.4846 | 0.4805 | 0.107* | |
H9B | 0.4235 | 0.4055 | 0.5155 | 0.107* | |
C10 | 0.2266 (11) | 0.3990 (7) | 0.5692 (7) | 0.096 (3) | |
H10A | 0.1315 | 0.4081 | 0.5456 | 0.116* | |
H10B | 0.2416 | 0.4432 | 0.6184 | 0.116* | |
C11 | 0.2360 (10) | 0.3044 (7) | 0.6098 (6) | 0.087 (3) | |
H11A | 0.3327 | 0.2929 | 0.6292 | 0.104* | |
H11B | 0.1767 | 0.3015 | 0.6642 | 0.104* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0412 (6) | 0.0583 (7) | 0.0608 (7) | −0.0036 (6) | 0.0004 (5) | −0.0026 (6) |
Cl1 | 0.0592 (18) | 0.085 (2) | 0.0629 (17) | 0.0027 (17) | 0.0081 (14) | 0.0086 (16) |
Cl2 | 0.077 (2) | 0.081 (2) | 0.071 (2) | 0.0016 (18) | 0.0050 (16) | −0.0032 (17) |
N1 | 0.080 (5) | 0.094 (5) | 0.081 (5) | −0.015 (4) | 0.006 (4) | −0.003 (4) |
N2 | 0.054 (4) | 0.097 (5) | 0.082 (4) | −0.019 (4) | −0.012 (4) | −0.018 (4) |
N3 | 0.078 (5) | 0.076 (5) | 0.064 (5) | −0.001 (4) | −0.021 (5) | 0.002 (4) |
N4 | 0.062 (5) | 0.074 (6) | 0.072 (5) | 0.003 (4) | 0.010 (4) | −0.011 (4) |
N5 | 0.061 (5) | 0.068 (5) | 0.079 (5) | −0.010 (4) | −0.007 (4) | 0.003 (5) |
O1 | 0.052 (9) | 0.110 (12) | 0.114 (10) | −0.014 (9) | −0.009 (8) | 0.007 (10) |
O2 | 0.120 (14) | 0.107 (12) | 0.165 (13) | −0.012 (11) | 0.044 (12) | 0.023 (11) |
O3 | 0.089 (12) | 0.132 (14) | 0.117 (11) | −0.028 (11) | 0.065 (10) | −0.032 (11) |
O1' | 0.080 (10) | 0.099 (10) | 0.146 (10) | −0.017 (9) | 0.062 (8) | 0.038 (8) |
O2' | 0.115 (12) | 0.101 (11) | 0.127 (10) | −0.019 (9) | 0.039 (9) | −0.038 (9) |
O3' | 0.044 (7) | 0.134 (12) | 0.103 (8) | 0.026 (8) | 0.009 (6) | 0.011 (9) |
O4 | 0.085 (5) | 0.187 (6) | 0.082 (5) | 0.010 (4) | −0.011 (4) | 0.036 (4) |
O5 | 0.124 (9) | 0.147 (9) | 0.154 (9) | −0.044 (8) | 0.034 (7) | 0.046 (8) |
O6 | 0.154 (10) | 0.124 (8) | 0.115 (8) | 0.032 (8) | 0.000 (8) | 0.044 (7) |
O7 | 0.171 (10) | 0.156 (9) | 0.094 (7) | 0.038 (7) | −0.032 (7) | −0.054 (6) |
O8 | 0.101 (8) | 0.113 (8) | 0.185 (9) | 0.024 (7) | 0.074 (7) | −0.038 (7) |
O5' | 0.094 (13) | 0.124 (13) | 0.110 (12) | −0.021 (12) | −0.007 (12) | 0.016 (12) |
O6' | 0.106 (14) | 0.142 (14) | 0.174 (14) | 0.006 (13) | 0.056 (13) | −0.009 (14) |
O7' | 0.121 (14) | 0.114 (13) | 0.104 (13) | −0.026 (13) | 0.026 (13) | 0.049 (12) |
O8' | 0.127 (14) | 0.109 (14) | 0.108 (13) | 0.024 (13) | 0.014 (13) | −0.016 (12) |
C1 | 0.111 (7) | 0.084 (6) | 0.100 (6) | −0.043 (6) | 0.017 (6) | −0.005 (5) |
C2 | 0.077 (6) | 0.136 (7) | 0.120 (6) | −0.045 (6) | 0.005 (5) | −0.020 (6) |
C3 | 0.070 (5) | 0.131 (7) | 0.100 (6) | −0.017 (6) | 0.005 (5) | −0.016 (6) |
C4 | 0.068 (6) | 0.121 (7) | 0.088 (6) | 0.025 (6) | −0.022 (5) | −0.001 (6) |
C5 | 0.104 (7) | 0.093 (6) | 0.093 (6) | 0.007 (6) | −0.030 (6) | −0.004 (5) |
C6 | 0.163 (12) | 0.060 (7) | 0.065 (7) | −0.038 (8) | −0.018 (8) | 0.012 (6) |
C7 | 0.086 (9) | 0.156 (13) | 0.077 (8) | −0.048 (10) | 0.018 (7) | −0.011 (8) |
C8 | 0.056 (7) | 0.124 (10) | 0.088 (8) | −0.011 (7) | −0.003 (6) | −0.029 (8) |
C9 | 0.095 (9) | 0.058 (7) | 0.114 (9) | 0.001 (6) | −0.009 (7) | −0.027 (7) |
C10 | 0.099 (9) | 0.094 (9) | 0.097 (9) | 0.005 (8) | 0.015 (7) | −0.047 (7) |
C11 | 0.093 (8) | 0.110 (9) | 0.058 (7) | −0.011 (7) | 0.008 (6) | −0.006 (7) |
Ni1—N5 | 2.015 (6) | N5—C11 | 1.459 (9) |
Ni1—N4 | 2.026 (6) | N5—H5A | 0.9000 |
Ni1—N1 | 2.049 (6) | N5—H5B | 0.9000 |
Ni1—N2 | 2.058 (6) | C1—C2 | 1.472 (11) |
Ni1—N3 | 2.084 (7) | C1—H1C | 0.9700 |
Cl1—O2 | 1.35 (2) | C1—H1D | 0.9700 |
Cl1—O3 | 1.37 (2) | C2—C3 | 1.470 (11) |
Cl1—O4 | 1.394 (6) | C2—H2A | 0.9700 |
Cl1—O3' | 1.410 (11) | C2—H2B | 0.9700 |
Cl1—O2' | 1.411 (12) | C3—H3A | 0.9700 |
Cl1—O1' | 1.422 (11) | C3—H3B | 0.9700 |
Cl1—O1 | 1.435 (19) | C4—C5 | 1.439 (11) |
Cl2—O8 | 1.344 (9) | C4—H4C | 0.9700 |
Cl2—O6' | 1.354 (14) | C4—H4D | 0.9700 |
Cl2—O7 | 1.387 (9) | C5—H5C | 0.9700 |
Cl2—O7' | 1.389 (14) | C5—H5D | 0.9700 |
Cl2—O6 | 1.391 (9) | C6—C7 | 1.500 (12) |
Cl2—O5 | 1.398 (10) | C6—H6A | 0.9700 |
Cl2—O5' | 1.432 (14) | C6—H6B | 0.9700 |
Cl2—O8' | 1.471 (14) | C7—C8 | 1.476 (11) |
N1—C1 | 1.476 (9) | C7—H7A | 0.9700 |
N1—H1A | 0.9000 | C7—H7B | 0.9700 |
N1—H1B | 0.9000 | C8—H8A | 0.9700 |
N2—C3 | 1.422 (10) | C8—H8B | 0.9700 |
N2—C4 | 1.477 (10) | C9—C10 | 1.498 (11) |
N2—H2 | 0.9100 | C9—H9A | 0.9700 |
N3—C5 | 1.468 (10) | C9—H9B | 0.9700 |
N3—C9 | 1.494 (9) | C10—C11 | 1.502 (10) |
N3—C6 | 1.524 (11) | C10—H10A | 0.9700 |
N4—C8 | 1.462 (9) | C10—H10B | 0.9700 |
N4—H4A | 0.9000 | C11—H11A | 0.9700 |
N4—H4B | 0.9000 | C11—H11B | 0.9700 |
N5—Ni1—N4 | 99.5 (3) | N2—C3—H3A | 108.5 |
N5—Ni1—N1 | 97.8 (3) | C2—C3—H3A | 108.5 |
N4—Ni1—N1 | 90.3 (3) | N2—C3—H3B | 108.5 |
N5—Ni1—N2 | 97.7 (3) | C2—C3—H3B | 108.5 |
N4—Ni1—N2 | 162.4 (3) | H3A—C3—H3B | 107.5 |
N1—Ni1—N2 | 91.0 (3) | C5—C4—N2 | 109.6 (8) |
N5—Ni1—N3 | 96.3 (3) | C5—C4—H4C | 109.7 |
N4—Ni1—N3 | 90.7 (3) | N2—C4—H4C | 109.7 |
N1—Ni1—N3 | 165.5 (3) | C5—C4—H4D | 109.7 |
N2—Ni1—N3 | 83.8 (3) | N2—C4—H4D | 109.7 |
C1—N1—Ni1 | 119.8 (6) | H4C—C4—H4D | 108.2 |
C1—N1—H1A | 107.4 | C4—C5—N3 | 114.3 (8) |
Ni1—N1—H1A | 107.4 | C4—C5—H5C | 108.7 |
C1—N1—H1B | 107.4 | N3—C5—H5C | 108.7 |
Ni1—N1—H1B | 107.4 | C4—C5—H5D | 108.7 |
H1A—N1—H1B | 106.9 | N3—C5—H5D | 108.7 |
C3—N2—C4 | 116.3 (8) | H5C—C5—H5D | 107.6 |
C3—N2—Ni1 | 120.0 (6) | C7—C6—N3 | 115.3 (8) |
C4—N2—Ni1 | 105.5 (5) | C7—C6—H6A | 108.4 |
C3—N2—H2 | 104.4 | N3—C6—H6A | 108.4 |
C4—N2—H2 | 104.4 | C7—C6—H6B | 108.4 |
Ni1—N2—H2 | 104.4 | N3—C6—H6B | 108.4 |
C5—N3—C9 | 109.6 (7) | H6A—C6—H6B | 107.5 |
C5—N3—C6 | 107.4 (8) | C8—C7—C6 | 117.1 (9) |
C9—N3—C6 | 106.8 (7) | C8—C7—H7A | 108.0 |
C5—N3—Ni1 | 107.2 (6) | C6—C7—H7A | 108.0 |
C9—N3—Ni1 | 114.9 (5) | C8—C7—H7B | 108.0 |
C6—N3—Ni1 | 110.8 (5) | C6—C7—H7B | 108.0 |
C8—N4—Ni1 | 113.7 (5) | H7A—C7—H7B | 107.3 |
C8—N4—H4A | 108.8 | N4—C8—C7 | 111.3 (8) |
Ni1—N4—H4A | 108.8 | N4—C8—H8A | 109.4 |
C8—N4—H4B | 108.8 | C7—C8—H8A | 109.4 |
Ni1—N4—H4B | 108.8 | N4—C8—H8B | 109.4 |
H4A—N4—H4B | 107.7 | C7—C8—H8B | 109.4 |
C11—N5—Ni1 | 120.0 (5) | H8A—C8—H8B | 108.0 |
C11—N5—H5A | 107.3 | N3—C9—C10 | 116.7 (8) |
Ni1—N5—H5A | 107.3 | N3—C9—H9A | 108.1 |
C11—N5—H5B | 107.3 | C10—C9—H9A | 108.1 |
Ni1—N5—H5B | 107.3 | N3—C9—H9B | 108.1 |
H5A—N5—H5B | 106.9 | C10—C9—H9B | 108.1 |
C2—C1—N1 | 113.3 (8) | H9A—C9—H9B | 107.3 |
C2—C1—H1C | 108.9 | C9—C10—C11 | 115.6 (8) |
N1—C1—H1C | 108.9 | C9—C10—H10A | 108.4 |
C2—C1—H1D | 108.9 | C11—C10—H10A | 108.4 |
N1—C1—H1D | 108.9 | C9—C10—H10B | 108.4 |
H1C—C1—H1D | 107.7 | C11—C10—H10B | 108.4 |
C3—C2—C1 | 116.8 (9) | H10A—C10—H10B | 107.4 |
C3—C2—H2A | 108.1 | N5—C11—C10 | 113.0 (7) |
C1—C2—H2A | 108.1 | N5—C11—H11A | 109.0 |
C3—C2—H2B | 108.1 | C10—C11—H11A | 109.0 |
C1—C2—H2B | 108.1 | N5—C11—H11B | 109.0 |
H2A—C2—H2B | 107.3 | C10—C11—H11B | 109.0 |
N2—C3—C2 | 115.3 (9) | H11A—C11—H11B | 107.8 |
N5—Ni1—N1—C1 | 63.7 (7) | N4—Ni1—N5—C11 | 61.2 (6) |
N4—Ni1—N1—C1 | 163.4 (6) | N1—Ni1—N5—C11 | 152.8 (6) |
N2—Ni1—N1—C1 | −34.2 (7) | N2—Ni1—N5—C11 | −115.1 (6) |
N3—Ni1—N1—C1 | −102.9 (13) | N3—Ni1—N5—C11 | −30.6 (6) |
N5—Ni1—N2—C3 | −64.0 (7) | Ni1—N1—C1—C2 | 52.1 (10) |
N4—Ni1—N2—C3 | 128.2 (9) | N1—C1—C2—C3 | −64.4 (12) |
N1—Ni1—N2—C3 | 34.0 (7) | C4—N2—C3—C2 | 178.9 (8) |
N3—Ni1—N2—C3 | −159.6 (7) | Ni1—N2—C3—C2 | −52.0 (11) |
N5—Ni1—N2—C4 | 69.7 (6) | C1—C2—C3—N2 | 65.3 (12) |
N4—Ni1—N2—C4 | −98.1 (10) | C3—N2—C4—C5 | −178.8 (8) |
N1—Ni1—N2—C4 | 167.7 (6) | Ni1—N2—C4—C5 | 45.5 (9) |
N3—Ni1—N2—C4 | −25.8 (6) | N2—C4—C5—N3 | −47.2 (11) |
N5—Ni1—N3—C5 | −94.5 (6) | C9—N3—C5—C4 | −102.1 (10) |
N4—Ni1—N3—C5 | 165.8 (6) | C6—N3—C5—C4 | 142.3 (8) |
N1—Ni1—N3—C5 | 72.1 (14) | Ni1—N3—C5—C4 | 23.2 (10) |
N2—Ni1—N3—C5 | 2.6 (6) | C5—N3—C6—C7 | −174.4 (8) |
N5—Ni1—N3—C9 | 27.5 (6) | C9—N3—C6—C7 | 68.2 (10) |
N4—Ni1—N3—C9 | −72.2 (6) | Ni1—N3—C6—C7 | −57.6 (9) |
N1—Ni1—N3—C9 | −165.9 (10) | N3—C6—C7—C8 | 62.6 (12) |
N2—Ni1—N3—C9 | 124.6 (6) | Ni1—N4—C8—C7 | 66.9 (9) |
N5—Ni1—N3—C6 | 148.6 (6) | C6—C7—C8—N4 | −65.3 (12) |
N4—Ni1—N3—C6 | 48.9 (6) | C5—N3—C9—C10 | 72.8 (10) |
N1—Ni1—N3—C6 | −44.7 (14) | C6—N3—C9—C10 | −171.2 (8) |
N2—Ni1—N3—C6 | −114.3 (6) | Ni1—N3—C9—C10 | −47.9 (10) |
N5—Ni1—N4—C8 | −152.0 (6) | N3—C9—C10—C11 | 68.4 (11) |
N1—Ni1—N4—C8 | 110.1 (6) | Ni1—N5—C11—C10 | 50.8 (10) |
N2—Ni1—N4—C8 | 15.8 (12) | C9—C10—C11—N5 | −67.6 (11) |
N3—Ni1—N4—C8 | −55.5 (6) |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O4 | 0.90 | 2.52 | 3.119 (9) | 125 |
N1—H1B···O5′ | 0.90 | 2.22 | 2.95 (2) | 138 |
N1—H1B···O7 | 0.90 | 2.29 | 3.150 (13) | 160 |
N2—H2···O3′ | 0.91 | 2.34 | 3.24 (2) | 166 |
N2—H2···O4 | 0.91 | 2.51 | 3.161 (10) | 129 |
N2—H2···Cl1 | 0.91 | 2.95 | 3.801 (8) | 157 |
N4—H4A···O3′i | 0.90 | 2.32 | 3.140 (17) | 151 |
N4—H4A···O1i | 0.90 | 2.47 | 3.29 (3) | 153 |
N4—H4B···O7ii | 0.90 | 2.43 | 3.235 (13) | 149 |
N4—H4B···O6′ii | 0.90 | 2.64 | 3.42 (3) | 145 |
N4—H4B···O5 | 0.90 | 2.66 | 3.107 (12) | 112 |
N5—H5A···O1′iii | 0.90 | 2.31 | 3.14 (2) | 153 |
N5—H5A···O3iii | 0.90 | 2.54 | 3.33 (3) | 147 |
N5—H5B···O8′ | 0.90 | 2.23 | 2.95 (2) | 136 |
N5—H5B···O5′ | 0.90 | 2.45 | 3.30 (3) | 158 |
N5—H5B···O8 | 0.90 | 2.47 | 3.328 (14) | 160 |
N5—H5B···Cl2 | 0.90 | 2.94 | 3.794 (7) | 159 |
Symmetry codes: (i) x+1/2, −y+1/2, z+1/2; (ii) −x+1, −y, −z+1; (iii) x−1/2, −y+1/2, z+1/2. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register