Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807033296/xu2291sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807033296/xu2291Isup2.hkl |
CCDC reference: 657566
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.013 Å
- R factor = 0.056
- wR factor = 0.165
- Data-to-parameter ratio = 17.8
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT111_ALERT_2_B ADDSYM Detects (Pseudo) Centre of Symmetry ..... 100 PerFi PLAT112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... n
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT113_ALERT_2_C ADDSYM Suggests Possible Pseudo/New Spacegroup . P21/c PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.05 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.24 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C43 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C49 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C22 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C56 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C33 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C41 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C47 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C50 PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 13 PLAT420_ALERT_2_C D-H Without Acceptor N5 - H5B ... ? PLAT420_ALERT_2_C D-H Without Acceptor N7 - H7A ... ? PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4 PLAT731_ALERT_1_C Bond Calc 1.338(14), Rep 1.338(5) ...... 2.80 su-Ra N1 -C9 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.358(11), Rep 1.358(4) ...... 2.75 su-Ra N1 -C1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.333(13), Rep 1.332(5) ...... 2.60 su-Ra N2 -C12 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.365(11), Rep 1.365(4) ...... 2.75 su-Ra N2 -C6 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.337(12), Rep 1.339(5) ...... 2.40 su-Ra N3 -C21 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.360(9), Rep 1.360(4) ...... 2.25 su-Ra N3 -C13 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.338(12), Rep 1.340(5) ...... 2.40 su-Ra N4 -C24 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.463(11), Rep 1.464(5) ...... 2.20 su-Ra N7 -C39 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.335(14), Rep 1.334(5) ...... 2.80 su-Ra N9 -C61 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.364(11), Rep 1.364(4) ...... 2.75 su-Ra N9 -C53 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.337(15), Rep 1.337(5) ...... 3.00 su-Ra N10 -C64 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.364(11), Rep 1.364(4) ...... 2.75 su-Ra N10 -C58 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.343(13), Rep 1.342(5) ...... 2.60 su-Ra N11 -C73 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.365(10), Rep 1.365(4) ...... 2.50 su-Ra N11 -C65 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.340(13), Rep 1.340(5) ...... 2.60 su-Ra N12 -C76 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.391(11), Rep 1.390(5) ...... 2.20 su-Ra C2 -C7 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.386(11), Rep 1.386(5) ...... 2.20 su-Ra C5 -C10 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.376(16), Rep 1.376(5) ...... 3.20 su-Ra C7 -C8 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.387(16), Rep 1.386(5) ...... 3.20 su-Ra C8 -C9 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.385(17), Rep 1.384(5) ...... 3.40 su-Ra C10 -C11 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.395(16), Rep 1.396(5) ...... 3.20 su-Ra C11 -C12 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.403(11), Rep 1.403(5) ...... 2.20 su-Ra C14 -C19 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.397(12), Rep 1.397(5) ...... 2.40 su-Ra C17 -C22 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.385(14), Rep 1.384(5) ...... 2.80 su-Ra C19 -C20 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.387(13), Rep 1.387(5) ...... 2.60 su-Ra C20 -C21 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.380(14), Rep 1.380(5) ...... 2.80 su-Ra C22 -C23 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.393(15), Rep 1.393(5) ...... 3.00 su-Ra C23 -C24 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.514(9), Rep 1.515(4) ...... 2.25 su-Ra C25 -C27 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.514(10), Rep 1.514(4) ...... 2.50 su-Ra C26 -C33 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.390(11), Rep 1.391(5) ...... 2.20 su-Ra C54 -C59 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.390(11), Rep 1.389(5) ...... 2.20 su-Ra C57 -C62 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.378(18), Rep 1.377(5) ...... 3.60 su-Ra C59 -C60 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.388(17), Rep 1.388(5) ...... 3.40 su-Ra C60 -C61 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.381(16), Rep 1.381(5) ...... 3.20 su-Ra C62 -C63 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.395(17), Rep 1.395(5) ...... 3.40 su-Ra C63 -C64 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.397(12), Rep 1.395(5) ...... 2.40 su-Ra C66 -C71 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.398(12), Rep 1.398(5) ...... 2.40 su-Ra C69 -C74 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.378(15), Rep 1.379(5) ...... 3.00 su-Ra C71 -C72 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.386(14), Rep 1.387(5) ...... 2.80 su-Ra C72 -C73 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.377(14), Rep 1.377(5) ...... 2.80 su-Ra C74 -C75 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 1.392(16), Rep 1.393(5) ...... 3.20 su-Ra C75 -C76 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 27.50 From the CIF: _reflns_number_total 14184 Count of symmetry unique reflns 8518 Completeness (_total/calc) 166.52% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 5666 Fraction of Friedel pairs measured 0.665 Are heavy atom types Z>Si present yes PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT791_ALERT_1_G Confirm the Absolute Configuration of C25 = . R PLAT791_ALERT_1_G Confirm the Absolute Configuration of C26 = . R PLAT791_ALERT_1_G Confirm the Absolute Configuration of C39 = . R PLAT791_ALERT_1_G Confirm the Absolute Configuration of C40 = . R PLAT794_ALERT_5_G Check Predicted Bond Valency for Ni1 (2) 2.05 PLAT794_ALERT_5_G Check Predicted Bond Valency for Ni3 (2) 2.11 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 590
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 57 ALERT level C = Check and explain 10 ALERT level G = General alerts; check 48 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 14 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 2 ALERT type 4 Improvement, methodology, query or suggestion 2 ALERT type 5 Informative message, check
For the nickel complexes of meso-, R,R- and S,S -1,2-diphenylethylenediamine, see: Finney et al. (1981); García-Granda & Gómez-Beltrán (1984); García-Granda et al. (1990); Murmann & Barnes (2004).
Nickel chloride hexahydrate (0.237 g, 1 mmol), (1R,2R)-(+)–1,2-diphenylethylenediamine (0.212 g, 1 mmol) and 1,10-phenanthroline (0.198 g, 1 mmol) were placed in a 23-ml, Teflon-lined, Parr bomb along with ethanol (12 ml). The bomb was heated at 413 K for 72 h, and then cooled over 24 h. Green crystals were isolated in 40% yield.
The phenyl rings were refined as rigid hexagons of 1.39 Å sides as were the six-membered central ring in the phenanthroline ligands. In the phenanthroline ligands, the N–C distances were restrained to with 0.005 Å of each other, as were the other C–C distances. For the diphenylethylenediamine ligands, the N–C distances were restrained to 1.450±0.005 Å and the aliphatic C–C distances to 1.500±0.005 Å. Additionally, the temperature factors of all carbon, nitrogen and oxygen atoms were restrained to be nearly isotropic. The refinement necessitated somewhat tight restraints.
Carbon-bound H atoms were placed at calculated positions (C–H 0.93 Å) and were included in the refinement in the riding model approximation, with Uiso(H) set to 1.2 times Ueq(C). The water H-atoms were similarly treated (O–H 0.82 Å).
1,2-Diphenylethylenediamine, which can exist in the meso and the optically active R,R and S,S forms, behaves like ethylenediamine in a number of metal complexes; several nickel(II) complexes have been characterized by crystallography. These have the ligand functioning in the expected chelating mode, as noted in the nitrite/perchlorate, nitrite/chloride (Finney et al., 1981), dichloride (García-Granda & Gómez-Beltrán, 1984; Murmann & Barnes, 2004) and acetate (García-Granda et al., 1990) derivatives. The dichloride complexes are ionic and there is no direct interaction between the four-coordinate cation and the halide.
The attempt to synthesize a similar, mixed-ligand complex, by adding a molar equivalent of 1,10-phenanthroline yielded a cocrystal of dichlorobis(phenanthroline)nickel and diaquabis(diphenylethylenediamine)nickel dichloride (Fig. 1). The trinuclear compound lies on a false inversion site. The nickel atom of the diaquabis(diphenylethylenediamine)nickel cation lies on this site, which also relates the two neutral dichlorobis(phenanthroline)nickel to each other. The cation uses its water molecules to form hydrogen bonds to the free chlorine anion as well as to the chlorine atom of the neutral molecule. The three nickel atoms exist in octahedral geometries.
For the nickel complexes of meso-, R,R- and S,S -1,2-diphenylethylenediamine, see: Finney et al. (1981); García-Granda & Gómez-Beltrán (1984); García-Granda et al. (1990); Murmann & Barnes (2004).
Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).
[Ni(C14H16N2)2(H2O)2]Cl2·2[NiCl2(C12H8N2)2] | F(000) = 1620 |
Mr = 1570.25 | Dx = 1.461 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 3615 reflections |
a = 12.390 (2) Å | θ = 2.3–24.4° |
b = 13.819 (2) Å | µ = 1.06 mm−1 |
c = 21.261 (3) Å | T = 293 K |
β = 101.348 (2)° | Block, green |
V = 3569.1 (9) Å3 | 0.48 × 0.23 × 0.18 mm |
Z = 2 |
Bruker APEX area-detector diffractometer | 14184 independent reflections |
Radiation source: fine-focus sealed tube | 7201 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.046 |
φ and ω scans | θmax = 27.5°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −16→14 |
Tmin = 0.629, Tmax = 0.832 | k = −15→17 |
22161 measured reflections | l = −27→27 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.056 | H-atom parameters constrained |
wR(F2) = 0.165 | w = 1/[σ2(Fo2) + (0.0657P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.02 | (Δ/σ)max = 0.002 |
14184 reflections | Δρmax = 0.73 e Å−3 |
796 parameters | Δρmin = −0.50 e Å−3 |
590 restraints | Absolute structure: Flack (1983), 5767 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.07 (3) |
[Ni(C14H16N2)2(H2O)2]Cl2·2[NiCl2(C12H8N2)2] | V = 3569.1 (9) Å3 |
Mr = 1570.25 | Z = 2 |
Monoclinic, P21 | Mo Kα radiation |
a = 12.390 (2) Å | µ = 1.06 mm−1 |
b = 13.819 (2) Å | T = 293 K |
c = 21.261 (3) Å | 0.48 × 0.23 × 0.18 mm |
β = 101.348 (2)° |
Bruker APEX area-detector diffractometer | 14184 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 7201 reflections with I > 2σ(I) |
Tmin = 0.629, Tmax = 0.832 | Rint = 0.046 |
22161 measured reflections |
R[F2 > 2σ(F2)] = 0.056 | H-atom parameters constrained |
wR(F2) = 0.165 | Δρmax = 0.73 e Å−3 |
S = 1.02 | Δρmin = −0.50 e Å−3 |
14184 reflections | Absolute structure: Flack (1983), 5767 Friedel pairs |
796 parameters | Absolute structure parameter: −0.07 (3) |
590 restraints |
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 | ||
Ni1 | 0.29514 (10) | 0.5000 (1) | 0.49741 (6) | 0.0299 (4) | |
Ni2 | 0.25490 (14) | 0.5183 (2) | 0.75226 (8) | 0.0338 (2) | |
Ni3 | 0.20348 (10) | 0.53816 (7) | 1.00447 (6) | 0.0316 (4) | |
Cl1 | 0.2252 (2) | 0.6289 (3) | 0.55598 (13) | 0.0430 (8) | |
Cl2 | 0.4373 (2) | 0.4691 (3) | 0.58756 (13) | 0.0421 (9) | |
Cl3 | 0.2784 (3) | 0.4096 (3) | 0.94865 (13) | 0.0456 (9) | |
Cl4 | 0.0615 (2) | 0.5664 (3) | 0.91330 (13) | 0.0424 (9) | |
Cl5 | 0.2419 (3) | 0.2174 (3) | 0.73513 (16) | 0.0572 (11) | |
Cl6 | 0.2600 (3) | 0.8237 (3) | 0.76323 (16) | 0.0553 (10) | |
O1W | 0.1792 (6) | 0.4053 (7) | 0.7986 (3) | 0.044 (2) | |
H1W1 | 0.1761 | 0.4221 | 0.8352 | 0.065* | |
H1W2 | 0.2159 | 0.3556 | 0.8000 | 0.065* | |
O2W | 0.3293 (6) | 0.6312 (7) | 0.7052 (3) | 0.044 (2) | |
H2W1 | 0.3028 | 0.6307 | 0.6667 | 0.066* | |
H2W2 | 0.3175 | 0.6838 | 0.7204 | 0.066* | |
N1 | 0.3601 (6) | 0.3954 (7) | 0.4420 (4) | 0.038 (3) | |
N2 | 0.3986 (6) | 0.5863 (6) | 0.4543 (4) | 0.034 (3) | |
N3 | 0.1607 (5) | 0.5282 (6) | 0.4219 (3) | 0.030 (2) | |
N4 | 0.1767 (5) | 0.4016 (7) | 0.5181 (3) | 0.032 (2) | |
N5 | 0.1297 (5) | 0.4921 (7) | 0.6732 (4) | 0.035 (2) | |
H5A | 0.1451 | 0.5194 | 0.6397 | 0.042* | |
H5B | 0.1230 | 0.4310 | 0.6661 | 0.042* | |
N6 | 0.1413 (6) | 0.6165 (7) | 0.7728 (3) | 0.035 (2) | |
H6A | 0.1134 | 0.5957 | 0.8042 | 0.042* | |
H6B | 0.1731 | 0.6710 | 0.7838 | 0.042* | |
N7 | 0.3814 (6) | 0.5373 (7) | 0.8346 (4) | 0.042 (2) | |
H7A | 0.4106 | 0.5936 | 0.8335 | 0.051* | |
H7B | 0.3539 | 0.5339 | 0.8686 | 0.051* | |
N8 | 0.3740 (5) | 0.4240 (7) | 0.7278 (4) | 0.035 (2) | |
H8A | 0.3543 | 0.3650 | 0.7320 | 0.042* | |
H8B | 0.3785 | 0.4329 | 0.6884 | 0.042* | |
N9 | 0.1349 (6) | 0.6434 (7) | 1.0580 (4) | 0.038 (3) | |
N10 | 0.1035 (7) | 0.4532 (7) | 1.0484 (4) | 0.039 (3) | |
N11 | 0.3398 (5) | 0.5123 (7) | 1.0794 (4) | 0.034 (2) | |
N12 | 0.3175 (5) | 0.6347 (7) | 0.9814 (3) | 0.033 (2) | |
C1 | 0.4366 (5) | 0.4348 (6) | 0.4119 (3) | 0.037 (3) | |
C2 | 0.4929 (7) | 0.3789 (5) | 0.3745 (4) | 0.056 (4) | |
C3 | 0.5649 (6) | 0.4225 (8) | 0.3406 (3) | 0.076 (5) | |
H3 | 0.6025 | 0.3851 | 0.3156 | 0.092* | |
C4 | 0.5806 (5) | 0.5221 (8) | 0.3441 (3) | 0.070 (4) | |
H4 | 0.6288 | 0.5513 | 0.3214 | 0.084* | |
C5 | 0.5244 (7) | 0.5780 (5) | 0.3814 (4) | 0.054 (4) | |
C6 | 0.4524 (5) | 0.5344 (6) | 0.4153 (3) | 0.040 (3) | |
C7 | 0.4764 (10) | 0.2793 (6) | 0.3723 (6) | 0.072 (5) | |
H7 | 0.5165 | 0.2402 | 0.3496 | 0.086* | |
C8 | 0.4004 (9) | 0.2388 (9) | 0.4037 (5) | 0.066 (4) | |
H8 | 0.3877 | 0.1725 | 0.4025 | 0.079* | |
C9 | 0.3432 (10) | 0.2998 (7) | 0.4373 (5) | 0.054 (4) | |
H9 | 0.2904 | 0.2729 | 0.4576 | 0.065* | |
C10 | 0.5338 (10) | 0.6777 (6) | 0.3872 (6) | 0.070 (4) | |
H10 | 0.5800 | 0.7101 | 0.3647 | 0.084* | |
C11 | 0.4768 (9) | 0.7308 (10) | 0.4253 (5) | 0.071 (5) | |
H11 | 0.4836 | 0.7978 | 0.4277 | 0.086* | |
C12 | 0.4090 (9) | 0.6821 (7) | 0.4600 (5) | 0.049 (3) | |
H12 | 0.3716 | 0.7160 | 0.4869 | 0.059* | |
C13 | 0.0692 (5) | 0.4766 (5) | 0.4267 (3) | 0.031 (3) | |
C14 | −0.0298 (6) | 0.4863 (5) | 0.3832 (3) | 0.034 (3) | |
C15 | −0.1196 (4) | 0.4293 (7) | 0.3894 (3) | 0.055 (4) | |
H15 | −0.1858 | 0.4358 | 0.3602 | 0.066* | |
C16 | −0.1104 (5) | 0.3626 (6) | 0.4390 (4) | 0.048 (3) | |
H16 | −0.1704 | 0.3244 | 0.4432 | 0.057* | |
C17 | −0.0114 (6) | 0.3529 (5) | 0.4826 (3) | 0.041 (3) | |
C18 | 0.0784 (4) | 0.4099 (6) | 0.4764 (3) | 0.033 (3) | |
C19 | −0.0362 (8) | 0.5558 (7) | 0.3345 (4) | 0.046 (3) | |
H19 | −0.1014 | 0.5652 | 0.3049 | 0.055* | |
C20 | 0.0565 (7) | 0.6102 (9) | 0.3315 (5) | 0.049 (4) | |
H20 | 0.0538 | 0.6570 | 0.2998 | 0.059* | |
C21 | 0.1533 (8) | 0.5951 (8) | 0.3758 (4) | 0.045 (3) | |
H21 | 0.2148 | 0.6324 | 0.3732 | 0.054* | |
C22 | 0.0032 (9) | 0.2872 (8) | 0.5335 (4) | 0.061 (4) | |
H22 | −0.0558 | 0.2487 | 0.5389 | 0.073* | |
C23 | 0.1023 (7) | 0.2777 (9) | 0.5760 (5) | 0.046 (3) | |
H23 | 0.1114 | 0.2333 | 0.6095 | 0.055* | |
C24 | 0.1879 (8) | 0.3376 (8) | 0.5662 (4) | 0.040 (3) | |
H24 | 0.2555 | 0.3330 | 0.5943 | 0.048* | |
C25 | 0.0271 (5) | 0.5315 (5) | 0.6866 (3) | 0.042 (2) | |
H25 | 0.0064 | 0.4906 | 0.7200 | 0.051* | |
C26 | 0.0539 (5) | 0.6301 (5) | 0.7160 (3) | 0.041 (2) | |
H26 | 0.0874 | 0.6664 | 0.6852 | 0.049* | |
C27 | −0.0695 (5) | 0.5310 (6) | 0.6305 (3) | 0.042 (3) | |
C28 | −0.1636 (6) | 0.4801 (6) | 0.6368 (3) | 0.068 (3) | |
H28 | −0.1660 | 0.4473 | 0.6747 | 0.082* | |
C29 | −0.2541 (5) | 0.4781 (6) | 0.5864 (4) | 0.072 (3) | |
H29 | −0.3170 | 0.4440 | 0.5906 | 0.086* | |
C30 | −0.2505 (5) | 0.5271 (7) | 0.5297 (3) | 0.067 (3) | |
H30 | −0.3110 | 0.5258 | 0.4960 | 0.081* | |
C31 | −0.1564 (6) | 0.5780 (6) | 0.5235 (3) | 0.064 (3) | |
H31 | −0.1540 | 0.6108 | 0.4856 | 0.077* | |
C32 | −0.0659 (5) | 0.5800 (6) | 0.5739 (3) | 0.056 (3) | |
H32 | −0.0030 | 0.6140 | 0.5697 | 0.067* | |
C33 | −0.0425 (5) | 0.6905 (6) | 0.7272 (4) | 0.037 (3) | |
C34 | −0.1180 (6) | 0.6580 (5) | 0.7629 (3) | 0.062 (3) | |
H34 | −0.1112 | 0.5962 | 0.7806 | 0.074* | |
C35 | −0.2038 (5) | 0.7177 (7) | 0.7721 (3) | 0.072 (3) | |
H35 | −0.2544 | 0.6959 | 0.7959 | 0.086* | |
C36 | −0.2141 (6) | 0.8101 (6) | 0.7456 (4) | 0.074 (4) | |
H36 | −0.2715 | 0.8500 | 0.7518 | 0.089* | |
C37 | −0.1386 (7) | 0.8426 (5) | 0.7100 (4) | 0.062 (3) | |
H37 | −0.1455 | 0.9044 | 0.6923 | 0.075* | |
C38 | −0.0528 (5) | 0.7829 (6) | 0.7008 (3) | 0.062 (3) | |
H38 | −0.0023 | 0.8047 | 0.6769 | 0.074* | |
C39 | 0.4657 (5) | 0.4626 (6) | 0.8365 (3) | 0.040 (2) | |
H39 | 0.4373 | 0.4035 | 0.8529 | 0.048* | |
C40 | 0.4817 (5) | 0.4411 (6) | 0.7691 (3) | 0.042 (2) | |
H40 | 0.5130 | 0.4990 | 0.7531 | 0.050* | |
C41 | 0.5703 (5) | 0.4891 (6) | 0.8827 (3) | 0.046 (3) | |
C42 | 0.6388 (7) | 0.5615 (6) | 0.8674 (3) | 0.091 (4) | |
H42 | 0.6197 | 0.5946 | 0.8288 | 0.109* | |
C43 | 0.7357 (6) | 0.5843 (6) | 0.9100 (4) | 0.113 (5) | |
H43 | 0.7815 | 0.6327 | 0.8998 | 0.136* | |
C44 | 0.7641 (5) | 0.5349 (7) | 0.9678 (4) | 0.079 (4) | |
H44 | 0.8290 | 0.5502 | 0.9963 | 0.095* | |
C45 | 0.6957 (6) | 0.4625 (6) | 0.9831 (3) | 0.073 (4) | |
H45 | 0.7147 | 0.4294 | 1.0217 | 0.087* | |
C46 | 0.5988 (6) | 0.4396 (5) | 0.9405 (3) | 0.056 (3) | |
H46 | 0.5530 | 0.3912 | 0.9507 | 0.067* | |
C47 | 0.5609 (5) | 0.3586 (5) | 0.7668 (4) | 0.041 (3) | |
C48 | 0.6560 (6) | 0.3785 (5) | 0.7438 (4) | 0.079 (4) | |
H48 | 0.6689 | 0.4409 | 0.7305 | 0.095* | |
C49 | 0.7318 (5) | 0.3054 (7) | 0.7407 (4) | 0.098 (5) | |
H49 | 0.7955 | 0.3188 | 0.7253 | 0.117* | |
C50 | 0.7125 (6) | 0.2123 (6) | 0.7606 (4) | 0.064 (3) | |
H50 | 0.7632 | 0.1634 | 0.7585 | 0.077* | |
C51 | 0.6174 (7) | 0.1923 (5) | 0.7836 (3) | 0.064 (4) | |
H51 | 0.6045 | 0.1300 | 0.7969 | 0.077* | |
C52 | 0.5416 (5) | 0.2654 (6) | 0.7867 (3) | 0.055 (3) | |
H52 | 0.4779 | 0.2520 | 0.8021 | 0.066* | |
C53 | 0.0607 (5) | 0.6031 (6) | 1.0899 (3) | 0.041 (3) | |
C54 | 0.0013 (7) | 0.6585 (5) | 1.1258 (4) | 0.056 (4) | |
C55 | −0.0704 (6) | 0.6138 (7) | 1.1595 (3) | 0.066 (4) | |
H55 | −0.1101 | 0.6508 | 1.1836 | 0.079* | |
C56 | −0.0827 (5) | 0.5138 (8) | 1.1572 (3) | 0.076 (4) | |
H56 | −0.1307 | 0.4839 | 1.1797 | 0.091* | |
C57 | −0.0233 (7) | 0.4585 (5) | 1.1212 (4) | 0.054 (4) | |
C58 | 0.0484 (5) | 0.5031 (6) | 1.0876 (3) | 0.041 (3) | |
C59 | 0.0182 (10) | 0.7580 (6) | 1.1268 (6) | 0.076 (5) | |
H59 | −0.0218 | 0.7974 | 1.1493 | 0.091* | |
C60 | 0.0933 (10) | 0.7992 (10) | 1.0949 (6) | 0.077 (5) | |
H60 | 0.1048 | 0.8657 | 1.0959 | 0.092* | |
C61 | 0.1513 (10) | 0.7389 (7) | 1.0612 (5) | 0.054 (4) | |
H61 | 0.2033 | 0.7658 | 1.0403 | 0.065* | |
C62 | −0.0342 (10) | 0.3584 (6) | 1.1188 (6) | 0.070 (4) | |
H62 | −0.0775 | 0.3266 | 1.1434 | 0.083* | |
C63 | 0.0209 (9) | 0.3075 (9) | 1.0789 (5) | 0.062 (4) | |
H63 | 0.0136 | 0.2407 | 1.0753 | 0.075* | |
C64 | 0.0877 (10) | 0.3575 (8) | 1.0442 (6) | 0.056 (4) | |
H64 | 0.1230 | 0.3224 | 1.0169 | 0.067* | |
C65 | 0.4298 (5) | 0.5649 (5) | 1.0721 (3) | 0.032 (3) | |
C66 | 0.5300 (6) | 0.5571 (5) | 1.1147 (3) | 0.044 (3) | |
C67 | 0.6183 (4) | 0.6146 (7) | 1.1068 (3) | 0.049 (3) | |
H67 | 0.6854 | 0.6094 | 1.1354 | 0.059* | |
C68 | 0.6065 (5) | 0.6800 (6) | 1.0563 (4) | 0.059 (4) | |
H68 | 0.6656 | 0.7186 | 1.0510 | 0.071* | |
C69 | 0.5063 (6) | 0.6879 (6) | 1.0136 (3) | 0.039 (3) | |
C70 | 0.4180 (4) | 0.6303 (6) | 1.0215 (3) | 0.031 (3) | |
C71 | 0.5383 (9) | 0.4863 (7) | 1.1623 (5) | 0.057 (4) | |
H71 | 0.6055 | 0.4764 | 1.1899 | 0.069* | |
C72 | 0.4489 (7) | 0.4308 (9) | 1.1691 (5) | 0.053 (4) | |
H72 | 0.4548 | 0.3836 | 1.2008 | 0.064* | |
C73 | 0.3498 (8) | 0.4475 (8) | 1.1273 (4) | 0.042 (3) | |
H73 | 0.2880 | 0.4126 | 1.1325 | 0.050* | |
C74 | 0.4920 (8) | 0.7537 (8) | 0.9627 (4) | 0.042 (3) | |
H74 | 0.5492 | 0.7938 | 0.9565 | 0.050* | |
C75 | 0.3907 (8) | 0.7573 (10) | 0.9221 (5) | 0.056 (4) | |
H75 | 0.3798 | 0.7985 | 0.8868 | 0.067* | |
C76 | 0.3046 (9) | 0.6995 (8) | 0.9336 (5) | 0.044 (3) | |
H76 | 0.2356 | 0.7061 | 0.9072 | 0.053* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0295 (7) | 0.0305 (11) | 0.0294 (7) | −0.0009 (7) | 0.0051 (6) | 0.0016 (8) |
Ni2 | 0.0321 (5) | 0.0401 (5) | 0.0297 (4) | −0.0037 (4) | 0.0073 (3) | −0.0004 (4) |
Ni3 | 0.0335 (8) | 0.0357 (12) | 0.0258 (7) | 0.0005 (7) | 0.0063 (6) | 0.0007 (8) |
Cl1 | 0.0495 (18) | 0.039 (2) | 0.0415 (17) | 0.0118 (15) | 0.0121 (14) | −0.0011 (16) |
Cl2 | 0.0401 (17) | 0.046 (2) | 0.0370 (16) | 0.0067 (15) | 0.0005 (13) | 0.0036 (16) |
Cl3 | 0.057 (2) | 0.045 (2) | 0.0348 (17) | 0.0134 (17) | 0.0100 (14) | −0.0015 (16) |
Cl4 | 0.0397 (17) | 0.050 (3) | 0.0343 (16) | 0.0065 (15) | 0.0002 (13) | 0.0008 (16) |
Cl5 | 0.061 (2) | 0.059 (3) | 0.0510 (18) | −0.0211 (19) | 0.0089 (16) | −0.007 (2) |
Cl6 | 0.070 (2) | 0.043 (3) | 0.0504 (18) | −0.0181 (19) | 0.0063 (17) | −0.0025 (19) |
O1W | 0.045 (4) | 0.053 (5) | 0.036 (4) | −0.004 (4) | 0.015 (3) | 0.008 (4) |
O2W | 0.054 (4) | 0.040 (5) | 0.041 (4) | −0.004 (4) | 0.015 (4) | 0.000 (4) |
N1 | 0.042 (5) | 0.042 (6) | 0.030 (5) | 0.000 (4) | 0.006 (4) | −0.005 (4) |
N2 | 0.032 (4) | 0.042 (6) | 0.029 (4) | −0.010 (4) | 0.003 (4) | 0.007 (4) |
N3 | 0.038 (4) | 0.026 (5) | 0.027 (4) | −0.004 (4) | 0.005 (3) | 0.002 (4) |
N4 | 0.038 (5) | 0.030 (5) | 0.031 (5) | −0.006 (4) | 0.010 (4) | −0.002 (4) |
N5 | 0.028 (4) | 0.035 (5) | 0.043 (4) | 0.003 (3) | 0.007 (3) | −0.002 (4) |
N6 | 0.032 (4) | 0.043 (5) | 0.029 (4) | −0.008 (4) | 0.004 (3) | −0.006 (4) |
N7 | 0.040 (4) | 0.052 (6) | 0.038 (4) | −0.004 (4) | 0.012 (3) | −0.006 (4) |
N8 | 0.033 (4) | 0.042 (5) | 0.033 (4) | 0.001 (4) | 0.012 (4) | 0.004 (4) |
N9 | 0.042 (5) | 0.039 (6) | 0.033 (5) | 0.006 (4) | 0.004 (4) | 0.002 (4) |
N10 | 0.033 (5) | 0.044 (6) | 0.037 (5) | −0.001 (4) | 0.006 (4) | 0.002 (5) |
N11 | 0.038 (4) | 0.038 (6) | 0.025 (4) | 0.005 (5) | 0.004 (3) | 0.003 (5) |
N12 | 0.038 (5) | 0.036 (6) | 0.023 (4) | 0.002 (4) | 0.002 (4) | 0.002 (4) |
C1 | 0.027 (5) | 0.050 (7) | 0.033 (5) | 0.008 (5) | 0.004 (4) | −0.002 (5) |
C2 | 0.046 (6) | 0.079 (8) | 0.040 (6) | 0.007 (6) | 0.004 (5) | −0.005 (6) |
C3 | 0.053 (7) | 0.125 (9) | 0.052 (7) | 0.016 (7) | 0.013 (6) | −0.014 (7) |
C4 | 0.042 (6) | 0.132 (9) | 0.043 (6) | −0.008 (7) | 0.022 (5) | 0.013 (7) |
C5 | 0.034 (5) | 0.085 (8) | 0.039 (6) | −0.008 (6) | −0.005 (5) | 0.002 (6) |
C6 | 0.031 (5) | 0.065 (7) | 0.026 (5) | 0.001 (5) | 0.009 (4) | 0.005 (5) |
C7 | 0.072 (7) | 0.090 (9) | 0.049 (6) | 0.028 (6) | 0.004 (6) | −0.022 (6) |
C8 | 0.082 (7) | 0.053 (7) | 0.058 (7) | 0.022 (6) | 0.005 (6) | −0.013 (6) |
C9 | 0.063 (6) | 0.052 (8) | 0.045 (6) | 0.003 (6) | 0.006 (5) | −0.004 (6) |
C10 | 0.056 (7) | 0.108 (9) | 0.044 (6) | −0.026 (6) | 0.004 (5) | 0.021 (6) |
C11 | 0.073 (7) | 0.062 (8) | 0.070 (7) | −0.027 (6) | −0.007 (6) | 0.025 (6) |
C12 | 0.048 (6) | 0.041 (7) | 0.053 (6) | −0.019 (5) | −0.004 (5) | 0.005 (5) |
C13 | 0.032 (5) | 0.030 (6) | 0.030 (5) | −0.003 (4) | 0.006 (4) | −0.004 (5) |
C14 | 0.029 (5) | 0.036 (6) | 0.034 (5) | 0.000 (4) | −0.002 (4) | −0.004 (5) |
C15 | 0.042 (6) | 0.064 (7) | 0.055 (6) | 0.002 (6) | 0.000 (5) | −0.014 (6) |
C16 | 0.032 (5) | 0.047 (7) | 0.060 (6) | −0.014 (5) | 0.002 (5) | −0.008 (5) |
C17 | 0.042 (6) | 0.040 (7) | 0.044 (6) | −0.011 (5) | 0.013 (5) | −0.002 (5) |
C18 | 0.029 (5) | 0.035 (6) | 0.034 (5) | −0.007 (5) | 0.009 (4) | −0.009 (5) |
C19 | 0.046 (6) | 0.056 (7) | 0.029 (5) | 0.007 (5) | −0.010 (4) | 0.002 (5) |
C20 | 0.053 (6) | 0.047 (7) | 0.044 (6) | 0.006 (5) | −0.001 (5) | 0.017 (6) |
C21 | 0.053 (6) | 0.049 (7) | 0.033 (5) | 0.005 (5) | 0.009 (5) | 0.005 (5) |
C22 | 0.058 (6) | 0.060 (8) | 0.069 (7) | −0.031 (6) | 0.025 (6) | −0.017 (6) |
C23 | 0.068 (6) | 0.038 (6) | 0.036 (5) | −0.010 (5) | 0.019 (5) | 0.005 (5) |
C24 | 0.045 (5) | 0.044 (7) | 0.029 (5) | 0.010 (5) | 0.003 (4) | 0.000 (5) |
C25 | 0.036 (4) | 0.050 (5) | 0.037 (4) | −0.002 (4) | −0.001 (3) | −0.002 (4) |
C26 | 0.034 (4) | 0.051 (5) | 0.034 (4) | 0.003 (4) | −0.002 (4) | 0.002 (4) |
C27 | 0.036 (5) | 0.059 (6) | 0.030 (4) | −0.003 (4) | 0.003 (4) | −0.008 (4) |
C28 | 0.056 (6) | 0.091 (8) | 0.050 (6) | −0.022 (5) | −0.009 (5) | 0.008 (5) |
C29 | 0.046 (5) | 0.089 (7) | 0.072 (6) | −0.029 (5) | −0.012 (5) | 0.008 (6) |
C30 | 0.055 (6) | 0.085 (7) | 0.051 (6) | 0.000 (5) | −0.016 (5) | 0.002 (5) |
C31 | 0.063 (6) | 0.067 (7) | 0.057 (6) | 0.004 (5) | 0.000 (5) | 0.008 (5) |
C32 | 0.050 (5) | 0.057 (6) | 0.053 (6) | −0.009 (5) | −0.005 (5) | −0.007 (5) |
C33 | 0.028 (4) | 0.052 (6) | 0.030 (4) | 0.003 (4) | 0.004 (4) | −0.001 (4) |
C34 | 0.059 (6) | 0.057 (6) | 0.071 (6) | −0.002 (5) | 0.016 (5) | 0.018 (5) |
C35 | 0.050 (5) | 0.094 (8) | 0.076 (6) | −0.008 (5) | 0.024 (5) | 0.015 (6) |
C36 | 0.065 (7) | 0.089 (8) | 0.069 (7) | 0.030 (6) | 0.013 (6) | −0.006 (6) |
C37 | 0.063 (6) | 0.053 (7) | 0.075 (7) | 0.006 (5) | 0.021 (5) | 0.017 (6) |
C38 | 0.057 (6) | 0.060 (7) | 0.073 (6) | 0.015 (5) | 0.023 (5) | 0.010 (5) |
C39 | 0.039 (4) | 0.043 (5) | 0.035 (4) | 0.003 (4) | −0.001 (4) | −0.002 (4) |
C40 | 0.031 (4) | 0.053 (5) | 0.039 (5) | 0.000 (4) | 0.004 (4) | −0.002 (4) |
C41 | 0.041 (5) | 0.060 (6) | 0.034 (5) | −0.002 (4) | 0.004 (4) | −0.003 (5) |
C42 | 0.088 (7) | 0.121 (9) | 0.057 (6) | −0.057 (6) | −0.004 (5) | 0.024 (6) |
C43 | 0.100 (8) | 0.141 (10) | 0.093 (8) | −0.056 (7) | 0.005 (7) | 0.014 (7) |
C44 | 0.056 (6) | 0.098 (8) | 0.070 (7) | −0.006 (6) | −0.020 (5) | −0.013 (6) |
C45 | 0.077 (7) | 0.067 (7) | 0.065 (6) | 0.003 (5) | −0.008 (5) | −0.004 (5) |
C46 | 0.051 (5) | 0.067 (6) | 0.045 (5) | −0.009 (5) | −0.003 (4) | −0.001 (5) |
C47 | 0.032 (5) | 0.056 (6) | 0.031 (5) | −0.006 (4) | 0.000 (4) | 0.000 (4) |
C48 | 0.070 (6) | 0.070 (7) | 0.108 (8) | 0.013 (5) | 0.042 (6) | 0.033 (6) |
C49 | 0.090 (7) | 0.097 (8) | 0.120 (8) | 0.017 (6) | 0.055 (7) | 0.032 (7) |
C50 | 0.049 (6) | 0.077 (7) | 0.069 (6) | 0.022 (5) | 0.018 (5) | 0.018 (6) |
C51 | 0.075 (6) | 0.059 (7) | 0.060 (6) | 0.016 (5) | 0.017 (5) | 0.010 (6) |
C52 | 0.063 (6) | 0.056 (7) | 0.055 (5) | 0.006 (5) | 0.032 (5) | 0.003 (5) |
C53 | 0.034 (5) | 0.068 (8) | 0.021 (5) | 0.007 (5) | 0.002 (4) | 0.000 (5) |
C54 | 0.044 (6) | 0.084 (8) | 0.040 (6) | 0.020 (6) | 0.010 (5) | −0.008 (6) |
C55 | 0.038 (6) | 0.120 (9) | 0.046 (6) | 0.014 (6) | 0.021 (5) | −0.011 (6) |
C56 | 0.048 (6) | 0.133 (9) | 0.046 (6) | −0.009 (7) | 0.010 (5) | 0.004 (7) |
C57 | 0.040 (6) | 0.086 (8) | 0.038 (6) | −0.013 (6) | 0.013 (5) | 0.012 (6) |
C58 | 0.031 (5) | 0.058 (7) | 0.033 (5) | −0.001 (5) | 0.001 (4) | 0.005 (5) |
C59 | 0.067 (7) | 0.097 (9) | 0.063 (7) | 0.035 (7) | 0.010 (6) | −0.021 (7) |
C60 | 0.096 (8) | 0.065 (8) | 0.070 (7) | 0.017 (7) | 0.015 (6) | −0.014 (7) |
C61 | 0.070 (7) | 0.047 (7) | 0.046 (6) | 0.007 (6) | 0.011 (5) | −0.012 (6) |
C62 | 0.051 (6) | 0.093 (8) | 0.059 (7) | −0.034 (6) | −0.002 (5) | 0.021 (6) |
C63 | 0.063 (7) | 0.052 (7) | 0.065 (7) | −0.024 (6) | −0.004 (6) | 0.012 (6) |
C64 | 0.058 (7) | 0.059 (8) | 0.048 (6) | −0.009 (6) | 0.006 (5) | −0.001 (6) |
C65 | 0.028 (5) | 0.034 (6) | 0.035 (5) | 0.006 (4) | 0.007 (4) | −0.008 (5) |
C66 | 0.044 (6) | 0.041 (7) | 0.046 (6) | 0.007 (5) | 0.002 (5) | −0.013 (5) |
C67 | 0.027 (5) | 0.050 (7) | 0.065 (6) | 0.004 (5) | −0.003 (5) | −0.007 (6) |
C68 | 0.050 (6) | 0.058 (7) | 0.074 (7) | −0.011 (6) | 0.021 (6) | −0.009 (6) |
C69 | 0.034 (5) | 0.044 (7) | 0.040 (5) | −0.002 (5) | 0.005 (4) | −0.003 (5) |
C70 | 0.035 (5) | 0.028 (6) | 0.028 (5) | 0.005 (5) | 0.001 (4) | 0.001 (5) |
C71 | 0.050 (6) | 0.064 (8) | 0.055 (6) | 0.016 (6) | 0.003 (5) | −0.011 (6) |
C72 | 0.064 (7) | 0.051 (7) | 0.039 (6) | 0.013 (6) | −0.002 (5) | 0.013 (6) |
C73 | 0.046 (6) | 0.039 (6) | 0.039 (5) | 0.001 (5) | 0.003 (5) | 0.005 (5) |
C74 | 0.048 (6) | 0.037 (6) | 0.042 (5) | −0.012 (5) | 0.011 (5) | 0.008 (5) |
C75 | 0.078 (7) | 0.042 (7) | 0.049 (6) | −0.012 (6) | 0.011 (6) | 0.006 (6) |
C76 | 0.050 (6) | 0.039 (7) | 0.042 (6) | −0.011 (5) | 0.007 (5) | 0.003 (5) |
Ni1—N2 | 2.090 (9) | C25—H25 | 0.9800 |
Ni1—N4 | 2.109 (8) | C26—C33 | 1.514 (4) |
Ni1—N3 | 2.109 (7) | C26—H26 | 0.9800 |
Ni1—N1 | 2.120 (10) | C27—C28 | 1.3900 |
Ni1—Cl2 | 2.372 (3) | C27—C32 | 1.3900 |
Ni1—Cl1 | 2.429 (3) | C28—C29 | 1.3900 |
Ni2—N6 | 2.064 (9) | C28—H28 | 0.9300 |
Ni2—N5 | 2.082 (8) | C29—C30 | 1.3900 |
Ni2—N8 | 2.108 (9) | C29—H29 | 0.9300 |
Ni2—N7 | 2.123 (8) | C30—C31 | 1.3900 |
Ni2—O1W | 2.157 (8) | C30—H30 | 0.9300 |
Ni2—O2W | 2.156 (8) | C31—C32 | 1.3900 |
Ni3—N10 | 2.059 (10) | C31—H31 | 0.9300 |
Ni3—N12 | 2.071 (9) | C32—H32 | 0.9300 |
Ni3—N11 | 2.112 (7) | C33—C34 | 1.3900 |
Ni3—N9 | 2.125 (10) | C33—C38 | 1.3900 |
Ni3—Cl4 | 2.380 (3) | C34—C35 | 1.3900 |
Ni3—Cl3 | 2.421 (4) | C34—H34 | 0.9300 |
O1W—H1W1 | 0.8200 | C35—C36 | 1.3900 |
O1W—H1W2 | 0.8200 | C35—H35 | 0.9300 |
O2W—H2W1 | 0.8200 | C36—C37 | 1.3900 |
O2W—H2W2 | 0.8200 | C36—H36 | 0.9300 |
N1—C9 | 1.338 (5) | C37—C38 | 1.3900 |
N1—C1 | 1.358 (4) | C37—H37 | 0.9300 |
N2—C12 | 1.332 (5) | C38—H38 | 0.9300 |
N2—C6 | 1.365 (4) | C39—C41 | 1.509 (5) |
N3—C21 | 1.339 (5) | C39—C40 | 1.515 (5) |
N3—C13 | 1.360 (4) | C39—H39 | 0.9800 |
N4—C24 | 1.340 (5) | C40—C47 | 1.511 (5) |
N4—C18 | 1.362 (4) | C40—H40 | 0.9800 |
N5—C25 | 1.462 (5) | C41—C42 | 1.3900 |
N5—H5A | 0.8600 | C41—C46 | 1.3900 |
N5—H5B | 0.8600 | C42—C43 | 1.3900 |
N6—C26 | 1.466 (5) | C42—H42 | 0.9300 |
N6—H6A | 0.8600 | C43—C44 | 1.3900 |
N6—H6B | 0.8600 | C43—H43 | 0.9300 |
N7—C39 | 1.464 (5) | C44—C45 | 1.3900 |
N7—H7A | 0.8600 | C44—H44 | 0.9300 |
N7—H7B | 0.8600 | C45—C46 | 1.3900 |
N8—C40 | 1.464 (5) | C45—H45 | 0.9300 |
N8—H8A | 0.8600 | C46—H46 | 0.9300 |
N8—H8B | 0.8600 | C47—C48 | 1.3900 |
N9—C61 | 1.334 (5) | C47—C52 | 1.3900 |
N9—C53 | 1.364 (4) | C48—C49 | 1.3900 |
N10—C64 | 1.337 (5) | C48—H48 | 0.9300 |
N10—C58 | 1.364 (4) | C49—C50 | 1.3900 |
N11—C73 | 1.342 (5) | C49—H49 | 0.9300 |
N11—C65 | 1.365 (4) | C50—C51 | 1.3900 |
N12—C76 | 1.340 (5) | C50—H50 | 0.9300 |
N12—C70 | 1.365 (4) | C51—C52 | 1.3900 |
C1—C2 | 1.3900 | C51—H51 | 0.9300 |
C1—C6 | 1.3900 | C52—H52 | 0.9300 |
C2—C7 | 1.390 (5) | C53—C54 | 1.3900 |
C2—C3 | 1.3900 | C53—C58 | 1.3900 |
C3—C4 | 1.3900 | C54—C55 | 1.3900 |
C3—H3 | 0.9300 | C54—C59 | 1.391 (5) |
C4—C5 | 1.3900 | C55—C56 | 1.3900 |
C4—H4 | 0.9300 | C55—H55 | 0.9300 |
C5—C10 | 1.386 (5) | C56—C57 | 1.3900 |
C5—C6 | 1.3900 | C56—H56 | 0.9300 |
C7—C8 | 1.376 (5) | C57—C62 | 1.389 (5) |
C7—H7 | 0.9300 | C57—C58 | 1.3900 |
C8—C9 | 1.386 (5) | C59—C60 | 1.377 (5) |
C8—H8 | 0.9300 | C59—H59 | 0.9300 |
C9—H9 | 0.9300 | C60—C61 | 1.388 (5) |
C10—C11 | 1.384 (5) | C60—H60 | 0.9300 |
C10—H10 | 0.9300 | C61—H61 | 0.9300 |
C11—C12 | 1.396 (5) | C62—C63 | 1.381 (5) |
C11—H11 | 0.9300 | C62—H62 | 0.9300 |
C12—H12 | 0.9300 | C63—C64 | 1.395 (5) |
C13—C14 | 1.3900 | C63—H63 | 0.9300 |
C13—C18 | 1.3900 | C64—H64 | 0.9300 |
C14—C15 | 1.3900 | C65—C66 | 1.3900 |
C14—C19 | 1.403 (5) | C65—C70 | 1.3900 |
C15—C16 | 1.3900 | C66—C67 | 1.3900 |
C15—H15 | 0.9300 | C66—C71 | 1.395 (5) |
C16—C17 | 1.3900 | C67—C68 | 1.3900 |
C16—H16 | 0.9300 | C67—H67 | 0.9300 |
C17—C18 | 1.3900 | C68—C69 | 1.3900 |
C17—C22 | 1.397 (5) | C68—H68 | 0.9300 |
C19—C20 | 1.384 (5) | C69—C70 | 1.3900 |
C19—H19 | 0.9300 | C69—C74 | 1.398 (5) |
C20—C21 | 1.387 (5) | C71—C72 | 1.379 (5) |
C20—H20 | 0.9300 | C71—H71 | 0.9300 |
C21—H21 | 0.9300 | C72—C73 | 1.387 (5) |
C22—C23 | 1.380 (5) | C72—H72 | 0.9300 |
C22—H22 | 0.9300 | C73—H73 | 0.9300 |
C23—C24 | 1.393 (5) | C74—C75 | 1.377 (5) |
C23—H23 | 0.9300 | C74—H74 | 0.9300 |
C24—H24 | 0.9300 | C75—C76 | 1.393 (5) |
C25—C26 | 1.508 (5) | C75—H75 | 0.9300 |
C25—C27 | 1.515 (4) | C76—H76 | 0.9300 |
N2—Ni1—N4 | 166.2 (3) | C23—C24—H24 | 118.7 |
N2—Ni1—N3 | 91.2 (3) | N5—C25—C26 | 106.7 (6) |
N4—Ni1—N3 | 78.4 (3) | N5—C25—C27 | 115.3 (6) |
N2—Ni1—N1 | 79.2 (3) | C26—C25—C27 | 114.0 (6) |
N4—Ni1—N1 | 91.9 (3) | N5—C25—H25 | 106.8 |
N3—Ni1—N1 | 91.9 (4) | C26—C25—H25 | 106.8 |
N2—Ni1—Cl2 | 92.0 (2) | C27—C25—H25 | 106.8 |
N4—Ni1—Cl2 | 98.76 (18) | N6—C26—C25 | 107.0 (6) |
N3—Ni1—Cl2 | 175.8 (2) | N6—C26—C33 | 114.8 (6) |
N1—Ni1—Cl2 | 91.4 (3) | C25—C26—C33 | 116.6 (6) |
N2—Ni1—Cl1 | 96.8 (2) | N6—C26—H26 | 105.9 |
N4—Ni1—Cl1 | 91.9 (3) | C25—C26—H26 | 105.9 |
N3—Ni1—Cl1 | 86.9 (3) | C33—C26—H26 | 105.9 |
N1—Ni1—Cl1 | 175.8 (2) | C28—C27—C32 | 120.0 |
Cl2—Ni1—Cl1 | 90.04 (12) | C28—C27—C25 | 118.3 (5) |
N6—Ni2—N5 | 81.6 (3) | C32—C27—C25 | 121.7 (6) |
N6—Ni2—N8 | 176.7 (5) | C27—C28—C29 | 120.0 |
N5—Ni2—N8 | 98.1 (3) | C27—C28—H28 | 120.0 |
N6—Ni2—N7 | 99.7 (3) | C29—C28—H28 | 120.0 |
N5—Ni2—N7 | 177.0 (5) | C30—C29—C28 | 120.0 |
N8—Ni2—N7 | 80.8 (3) | C30—C29—H29 | 120.0 |
N6—Ni2—O1W | 90.2 (3) | C28—C29—H29 | 120.0 |
N5—Ni2—O1W | 85.5 (3) | C29—C30—C31 | 120.0 |
N8—Ni2—O1W | 93.1 (3) | C29—C30—H30 | 120.0 |
N7—Ni2—O1W | 91.7 (3) | C31—C30—H30 | 120.0 |
N6—Ni2—O2W | 89.6 (4) | C32—C31—C30 | 120.0 |
N5—Ni2—O2W | 94.0 (3) | C32—C31—H31 | 120.0 |
N8—Ni2—O2W | 87.1 (3) | C30—C31—H31 | 120.0 |
N7—Ni2—O2W | 88.8 (3) | C31—C32—C27 | 120.0 |
O1W—Ni2—O2W | 179.5 (4) | C31—C32—H32 | 120.0 |
N10—Ni3—N12 | 166.9 (3) | C27—C32—H32 | 120.0 |
N10—Ni3—N11 | 91.4 (3) | C34—C33—C38 | 120.0 |
N12—Ni3—N11 | 78.8 (3) | C34—C33—C26 | 122.9 (6) |
N10—Ni3—N9 | 78.9 (3) | C38—C33—C26 | 117.1 (6) |
N12—Ni3—N9 | 92.8 (3) | C35—C34—C33 | 120.0 |
N11—Ni3—N9 | 93.2 (4) | C35—C34—H34 | 120.0 |
N10—Ni3—Cl4 | 92.8 (3) | C33—C34—H34 | 120.0 |
N12—Ni3—Cl4 | 97.50 (18) | C34—C35—C36 | 120.0 |
N11—Ni3—Cl4 | 174.6 (2) | C34—C35—H35 | 120.0 |
N9—Ni3—Cl4 | 90.8 (3) | C36—C35—H35 | 120.0 |
N10—Ni3—Cl3 | 97.3 (2) | C37—C36—C35 | 120.0 |
N12—Ni3—Cl3 | 90.6 (3) | C37—C36—H36 | 120.0 |
N11—Ni3—Cl3 | 85.4 (3) | C35—C36—H36 | 120.0 |
N9—Ni3—Cl3 | 175.9 (2) | C36—C37—C38 | 120.0 |
Cl4—Ni3—Cl3 | 90.83 (11) | C36—C37—H37 | 120.0 |
Ni2—O1W—H1W1 | 109.5 | C38—C37—H37 | 120.0 |
Ni2—O1W—H1W2 | 109.5 | C37—C38—C33 | 120.0 |
H1W1—O1W—H1W2 | 109.5 | C37—C38—H38 | 120.0 |
Ni2—O2W—H2W1 | 109.5 | C33—C38—H38 | 120.0 |
Ni2—O2W—H2W2 | 109.5 | N7—C39—C41 | 111.4 (6) |
H2W1—O2W—H2W2 | 109.5 | N7—C39—C40 | 109.7 (6) |
C9—N1—C1 | 118.3 (10) | C41—C39—C40 | 114.1 (6) |
C9—N1—Ni1 | 130.1 (7) | N7—C39—H39 | 107.1 |
C1—N1—Ni1 | 111.4 (7) | C41—C39—H39 | 107.1 |
C12—N2—C6 | 121.8 (10) | C40—C39—H39 | 107.1 |
C12—N2—Ni1 | 125.7 (7) | N8—C40—C47 | 112.4 (6) |
C6—N2—Ni1 | 112.4 (7) | N8—C40—C39 | 109.0 (5) |
C21—N3—C13 | 118.6 (8) | C47—C40—C39 | 112.6 (6) |
C21—N3—Ni1 | 128.0 (6) | N8—C40—H40 | 107.5 |
C13—N3—Ni1 | 113.1 (5) | C47—C40—H40 | 107.5 |
C24—N4—C18 | 119.8 (8) | C39—C40—H40 | 107.5 |
C24—N4—Ni1 | 127.8 (6) | C42—C41—C46 | 120.0 |
C18—N4—Ni1 | 112.4 (5) | C42—C41—C39 | 120.5 (6) |
C25—N5—Ni2 | 108.4 (5) | C46—C41—C39 | 119.5 (6) |
C25—N5—H5A | 110.0 | C43—C42—C41 | 120.0 |
Ni2—N5—H5A | 110.0 | C43—C42—H42 | 120.0 |
C25—N5—H5B | 110.0 | C41—C42—H42 | 120.0 |
Ni2—N5—H5B | 110.0 | C42—C43—C44 | 120.0 |
H5A—N5—H5B | 108.4 | C42—C43—H43 | 120.0 |
C26—N6—Ni2 | 109.5 (5) | C44—C43—H43 | 120.0 |
C26—N6—H6A | 109.8 | C45—C44—C43 | 120.0 |
Ni2—N6—H6A | 109.8 | C45—C44—H44 | 120.0 |
C26—N6—H6B | 109.8 | C43—C44—H44 | 120.0 |
Ni2—N6—H6B | 109.8 | C46—C45—C44 | 120.0 |
H6A—N6—H6B | 108.2 | C46—C45—H45 | 120.0 |
C39—N7—Ni2 | 110.1 (5) | C44—C45—H45 | 120.0 |
C39—N7—H7A | 109.6 | C45—C46—C41 | 120.0 |
Ni2—N7—H7A | 109.6 | C45—C46—H46 | 120.0 |
C39—N7—H7B | 109.6 | C41—C46—H46 | 120.0 |
Ni2—N7—H7B | 109.6 | C48—C47—C52 | 120.0 |
H7A—N7—H7B | 108.2 | C48—C47—C40 | 117.5 (6) |
C40—N8—Ni2 | 110.6 (5) | C52—C47—C40 | 122.5 (6) |
C40—N8—H8A | 109.5 | C47—C48—C49 | 120.0 |
Ni2—N8—H8A | 109.5 | C47—C48—H48 | 120.0 |
C40—N8—H8B | 109.5 | C49—C48—H48 | 120.0 |
Ni2—N8—H8B | 109.5 | C50—C49—C48 | 120.0 |
H8A—N8—H8B | 108.1 | C50—C49—H49 | 120.0 |
C61—N9—C53 | 119.3 (10) | C48—C49—H49 | 120.0 |
C61—N9—Ni3 | 129.1 (7) | C49—C50—C51 | 120.0 |
C53—N9—Ni3 | 111.5 (7) | C49—C50—H50 | 120.0 |
C64—N10—C58 | 117.1 (10) | C51—C50—H50 | 120.0 |
C64—N10—Ni3 | 128.9 (7) | C52—C51—C50 | 120.0 |
C58—N10—Ni3 | 114.0 (7) | C52—C51—H51 | 120.0 |
C73—N11—C65 | 119.1 (8) | C50—C51—H51 | 120.0 |
C73—N11—Ni3 | 128.7 (6) | C51—C52—C47 | 120.0 |
C65—N11—Ni3 | 111.9 (5) | C51—C52—H52 | 120.0 |
C76—N12—C70 | 117.5 (8) | C47—C52—H52 | 120.0 |
C76—N12—Ni3 | 128.7 (6) | N9—C53—C54 | 122.0 (8) |
C70—N12—Ni3 | 113.8 (6) | N9—C53—C58 | 118.0 (8) |
N1—C1—C2 | 121.4 (8) | C54—C53—C58 | 120.0 |
N1—C1—C6 | 118.4 (8) | C55—C54—C53 | 120.0 |
C2—C1—C6 | 120.0 | C55—C54—C59 | 122.8 (9) |
C7—C2—C1 | 118.9 (9) | C53—C54—C59 | 117.2 (9) |
C7—C2—C3 | 121.1 (9) | C54—C55—C56 | 120.0 |
C1—C2—C3 | 120.0 | C54—C55—H55 | 120.0 |
C4—C3—C2 | 120.0 | C56—C55—H55 | 120.0 |
C4—C3—H3 | 120.0 | C57—C56—C55 | 120.0 |
C2—C3—H3 | 120.0 | C57—C56—H56 | 120.0 |
C3—C4—C5 | 120.0 | C55—C56—H56 | 120.0 |
C3—C4—H4 | 120.0 | C62—C57—C56 | 120.7 (9) |
C5—C4—H4 | 120.0 | C62—C57—C58 | 119.3 (9) |
C10—C5—C6 | 115.9 (9) | C56—C57—C58 | 120.0 |
C10—C5—C4 | 124.1 (9) | N10—C58—C57 | 122.5 (8) |
C6—C5—C4 | 120.0 | N10—C58—C53 | 117.4 (8) |
N2—C6—C5 | 121.8 (8) | C57—C58—C53 | 120.0 |
N2—C6—C1 | 118.2 (8) | C60—C59—C54 | 121.1 (12) |
C5—C6—C1 | 120.0 | C60—C59—H59 | 119.5 |
C8—C7—C2 | 119.7 (11) | C54—C59—H59 | 119.5 |
C8—C7—H7 | 120.2 | C59—C60—C61 | 118.3 (13) |
C2—C7—H7 | 120.2 | C59—C60—H60 | 120.8 |
C7—C8—C9 | 118.1 (13) | C61—C60—H60 | 120.8 |
C7—C8—H8 | 121.0 | N9—C61—C60 | 122.1 (13) |
C9—C8—H8 | 121.0 | N9—C61—H61 | 119.0 |
N1—C9—C8 | 123.5 (13) | C60—C61—H61 | 119.0 |
N1—C9—H9 | 118.3 | C63—C62—C57 | 118.3 (11) |
C8—C9—H9 | 118.3 | C63—C62—H62 | 120.9 |
C11—C10—C5 | 122.4 (11) | C57—C62—H62 | 120.9 |
C11—C10—H10 | 118.8 | C62—C63—C64 | 119.3 (12) |
C5—C10—H10 | 118.8 | C62—C63—H63 | 120.4 |
C10—C11—C12 | 118.9 (12) | C64—C63—H63 | 120.4 |
C10—C11—H11 | 120.6 | N10—C64—C63 | 123.3 (12) |
C12—C11—H11 | 120.6 | N10—C64—H64 | 118.3 |
N2—C12—C11 | 119.2 (12) | C63—C64—H64 | 118.3 |
N2—C12—H12 | 120.4 | N11—C65—C66 | 121.9 (6) |
C11—C12—H12 | 120.4 | N11—C65—C70 | 118.1 (6) |
N3—C13—C14 | 122.6 (6) | C66—C65—C70 | 120.0 |
N3—C13—C18 | 117.3 (6) | C65—C66—C67 | 120.0 |
C14—C13—C18 | 120.0 | C65—C66—C71 | 117.2 (7) |
C13—C14—C15 | 120.0 | C67—C66—C71 | 122.7 (7) |
C13—C14—C19 | 118.1 (6) | C66—C67—C68 | 120.0 |
C15—C14—C19 | 121.8 (6) | C66—C67—H67 | 120.0 |
C16—C15—C14 | 120.0 | C68—C67—H67 | 120.0 |
C16—C15—H15 | 120.0 | C69—C68—C67 | 120.0 |
C14—C15—H15 | 120.0 | C69—C68—H68 | 120.0 |
C15—C16—C17 | 120.0 | C67—C68—H68 | 120.0 |
C15—C16—H16 | 120.0 | C68—C69—C70 | 120.0 |
C17—C16—H16 | 120.0 | C68—C69—C74 | 121.1 (7) |
C18—C17—C16 | 120.0 | C70—C69—C74 | 118.9 (7) |
C18—C17—C22 | 117.2 (6) | N12—C70—C69 | 122.8 (6) |
C16—C17—C22 | 122.8 (6) | N12—C70—C65 | 117.2 (6) |
N4—C18—C17 | 121.4 (6) | C69—C70—C65 | 120.0 |
N4—C18—C13 | 118.6 (6) | C72—C71—C66 | 121.3 (10) |
C17—C18—C13 | 120.0 | C72—C71—H71 | 119.3 |
C20—C19—C14 | 118.6 (9) | C66—C71—H71 | 119.3 |
C20—C19—H19 | 120.7 | C71—C72—C73 | 117.9 (11) |
C14—C19—H19 | 120.7 | C71—C72—H72 | 121.1 |
C19—C20—C21 | 120.1 (10) | C73—C72—H72 | 121.1 |
C19—C20—H20 | 119.9 | N11—C73—C72 | 122.3 (10) |
C21—C20—H20 | 119.9 | N11—C73—H73 | 118.8 |
N3—C21—C20 | 121.8 (10) | C72—C73—H73 | 118.8 |
N3—C21—H21 | 119.1 | C75—C74—C69 | 118.1 (9) |
C20—C21—H21 | 119.1 | C75—C74—H74 | 121.0 |
C23—C22—C17 | 122.1 (9) | C69—C74—H74 | 121.0 |
C23—C22—H22 | 118.9 | C74—C75—C76 | 120.3 (11) |
C17—C22—H22 | 118.9 | C74—C75—H75 | 119.9 |
C22—C23—C24 | 116.8 (10) | C76—C75—H75 | 119.9 |
C22—C23—H23 | 121.6 | N12—C76—C75 | 122.3 (10) |
C24—C23—H23 | 121.6 | N12—C76—H76 | 118.8 |
N4—C24—C23 | 122.6 (10) | C75—C76—H76 | 118.8 |
N4—C24—H24 | 118.7 | ||
N2—Ni1—N1—C9 | 177.9 (11) | C13—C14—C19—C20 | 1.0 (13) |
N4—Ni1—N1—C9 | −12.7 (11) | C15—C14—C19—C20 | 179.8 (8) |
N3—Ni1—N1—C9 | −91.1 (11) | C14—C19—C20—C21 | 0.4 (18) |
Cl2—Ni1—N1—C9 | 86.2 (11) | C13—N3—C21—C20 | −2.6 (16) |
N2—Ni1—N1—C1 | 3.7 (6) | Ni1—N3—C21—C20 | −175.3 (9) |
N4—Ni1—N1—C1 | 173.1 (6) | C19—C20—C21—N3 | 0.3 (18) |
N3—Ni1—N1—C1 | 94.6 (6) | C18—C17—C22—C23 | −0.7 (15) |
Cl2—Ni1—N1—C1 | −88.1 (6) | C16—C17—C22—C23 | 179.3 (10) |
N4—Ni1—N2—C12 | 125.7 (13) | C17—C22—C23—C24 | 0.6 (19) |
N3—Ni1—N2—C12 | 84.5 (10) | C18—N4—C24—C23 | 0.2 (17) |
N1—Ni1—N2—C12 | 176.1 (10) | Ni1—N4—C24—C23 | 178.4 (9) |
Cl2—Ni1—N2—C12 | −92.9 (9) | C22—C23—C24—N4 | −0.4 (19) |
Cl1—Ni1—N2—C12 | −2.6 (10) | Ni2—N5—C25—C26 | 44.3 (7) |
N4—Ni1—N2—C6 | −50.8 (16) | Ni2—N5—C25—C27 | 172.0 (5) |
N3—Ni1—N2—C6 | −92.1 (6) | Ni2—N6—C26—C25 | 41.4 (8) |
N1—Ni1—N2—C6 | −0.4 (6) | Ni2—N6—C26—C33 | 172.4 (6) |
Cl2—Ni1—N2—C6 | 90.6 (6) | N5—C25—C26—N6 | −56.9 (8) |
Cl1—Ni1—N2—C6 | −179.2 (6) | C27—C25—C26—N6 | 174.7 (6) |
N2—Ni1—N3—C21 | −12.3 (9) | N5—C25—C26—C33 | 173.2 (6) |
N4—Ni1—N3—C21 | 176.9 (10) | C27—C25—C26—C33 | 44.7 (9) |
N1—Ni1—N3—C21 | −91.6 (9) | N5—C25—C27—C28 | 120.6 (7) |
Cl1—Ni1—N3—C21 | 84.4 (9) | C26—C25—C27—C28 | −115.4 (6) |
N2—Ni1—N3—C13 | 174.6 (7) | N5—C25—C27—C32 | −59.6 (9) |
N4—Ni1—N3—C13 | 3.8 (6) | C26—C25—C27—C32 | 64.4 (8) |
N1—Ni1—N3—C13 | 95.4 (7) | C32—C27—C28—C29 | 0.0 |
Cl1—Ni1—N3—C13 | −88.7 (6) | C25—C27—C28—C29 | 179.8 (7) |
N2—Ni1—N4—C24 | 136.4 (12) | C27—C28—C29—C30 | 0.0 |
N3—Ni1—N4—C24 | 178.7 (10) | C28—C29—C30—C31 | 0.0 |
N1—Ni1—N4—C24 | 87.2 (10) | C29—C30—C31—C32 | 0.0 |
Cl2—Ni1—N4—C24 | −4.5 (9) | C30—C31—C32—C27 | 0.0 |
Cl1—Ni1—N4—C24 | −94.8 (9) | C28—C27—C32—C31 | 0.0 |
N2—Ni1—N4—C18 | −45.3 (17) | C25—C27—C32—C31 | −179.8 (7) |
N3—Ni1—N4—C18 | −3.0 (6) | N6—C26—C33—C34 | −70.8 (8) |
N1—Ni1—N4—C18 | −94.5 (7) | C25—C26—C33—C34 | 55.4 (8) |
Cl2—Ni1—N4—C18 | 173.8 (6) | N6—C26—C33—C38 | 108.3 (7) |
Cl1—Ni1—N4—C18 | 83.5 (6) | C25—C26—C33—C38 | −125.6 (6) |
N6—Ni2—N5—C25 | −17.4 (6) | C38—C33—C34—C35 | 0.0 |
N8—Ni2—N5—C25 | 166.0 (6) | C26—C33—C34—C35 | 179.1 (7) |
O1W—Ni2—N5—C25 | 73.5 (6) | C33—C34—C35—C36 | 0.0 |
O2W—Ni2—N5—C25 | −106.4 (6) | C34—C35—C36—C37 | 0.0 |
N5—Ni2—N6—C26 | −13.7 (6) | C35—C36—C37—C38 | 0.0 |
N7—Ni2—N6—C26 | 169.0 (6) | C36—C37—C38—C33 | 0.0 |
O1W—Ni2—N6—C26 | −99.2 (6) | C34—C33—C38—C37 | 0.0 |
O2W—Ni2—N6—C26 | 80.3 (6) | C26—C33—C38—C37 | −179.1 (6) |
N6—Ni2—N7—C39 | 170.6 (6) | Ni2—N7—C39—C41 | 164.2 (5) |
N8—Ni2—N7—C39 | −12.7 (6) | Ni2—N7—C39—C40 | 36.9 (8) |
O1W—Ni2—N7—C39 | 80.1 (6) | Ni2—N8—C40—C47 | 163.6 (5) |
O2W—Ni2—N7—C39 | −100.0 (6) | Ni2—N8—C40—C39 | 38.0 (8) |
N5—Ni2—N8—C40 | 168.5 (6) | N7—C39—C40—N8 | −49.8 (9) |
N7—Ni2—N8—C40 | −14.4 (6) | C41—C39—C40—N8 | −175.6 (7) |
O1W—Ni2—N8—C40 | −105.6 (6) | N7—C39—C40—C47 | −175.2 (7) |
O2W—Ni2—N8—C40 | 74.9 (6) | C41—C39—C40—C47 | 59.0 (9) |
N10—Ni3—N9—C61 | −179.0 (11) | N7—C39—C41—C42 | −73.0 (8) |
N12—Ni3—N9—C61 | 11.2 (11) | C40—C39—C41—C42 | 51.8 (8) |
N11—Ni3—N9—C61 | 90.2 (11) | N7—C39—C41—C46 | 107.8 (7) |
Cl4—Ni3—N9—C61 | −86.3 (10) | C40—C39—C41—C46 | −127.3 (6) |
N10—Ni3—N9—C53 | −2.5 (6) | C46—C41—C42—C43 | 0.0 |
N12—Ni3—N9—C53 | −172.2 (6) | C39—C41—C42—C43 | −179.1 (8) |
N11—Ni3—N9—C53 | −93.3 (6) | C41—C42—C43—C44 | 0.0 |
Cl4—Ni3—N9—C53 | 90.2 (6) | C42—C43—C44—C45 | 0.0 |
N12—Ni3—N10—C64 | −127.8 (14) | C43—C44—C45—C46 | 0.0 |
N11—Ni3—N10—C64 | −86.4 (11) | C44—C45—C46—C41 | 0.0 |
N9—Ni3—N10—C64 | −179.4 (11) | C42—C41—C46—C45 | 0.0 |
Cl4—Ni3—N10—C64 | 90.3 (10) | C39—C41—C46—C45 | 179.1 (7) |
Cl3—Ni3—N10—C64 | −0.9 (11) | N8—C40—C47—C48 | 117.7 (6) |
N12—Ni3—N10—C58 | 51.0 (17) | C39—C40—C47—C48 | −118.8 (6) |
N11—Ni3—N10—C58 | 92.3 (7) | N8—C40—C47—C52 | −62.3 (8) |
N9—Ni3—N10—C58 | −0.7 (6) | C39—C40—C47—C52 | 61.2 (8) |
Cl4—Ni3—N10—C58 | −91.0 (6) | C52—C47—C48—C49 | 0.0 |
Cl3—Ni3—N10—C58 | 177.8 (6) | C40—C47—C48—C49 | 180.0 (6) |
N10—Ni3—N11—C73 | 11.2 (10) | C47—C48—C49—C50 | 0.0 |
N12—Ni3—N11—C73 | −177.6 (10) | C48—C49—C50—C51 | 0.0 |
N9—Ni3—N11—C73 | 90.2 (10) | C49—C50—C51—C52 | 0.0 |
Cl3—Ni3—N11—C73 | −86.0 (10) | C50—C51—C52—C47 | 0.0 |
N10—Ni3—N11—C65 | −175.0 (7) | C48—C47—C52—C51 | 0.0 |
N12—Ni3—N11—C65 | −3.8 (6) | C40—C47—C52—C51 | −180.0 (7) |
N9—Ni3—N11—C65 | −96.0 (7) | C61—N9—C53—C54 | −0.1 (13) |
Cl3—Ni3—N11—C65 | 87.8 (6) | Ni3—N9—C53—C54 | −177.0 (3) |
N10—Ni3—N12—C76 | −134.3 (13) | C61—N9—C53—C58 | −177.7 (8) |
N11—Ni3—N12—C76 | −176.6 (11) | Ni3—N9—C53—C58 | 5.4 (8) |
N9—Ni3—N12—C76 | −83.9 (10) | N9—C53—C54—C55 | −177.5 (7) |
Cl4—Ni3—N12—C76 | 7.3 (10) | C58—C53—C54—C55 | 0.0 |
Cl3—Ni3—N12—C76 | 98.3 (10) | N9—C53—C54—C59 | 1.8 (9) |
N10—Ni3—N12—C70 | 45.0 (18) | C58—C53—C54—C59 | 179.3 (9) |
N11—Ni3—N12—C70 | 2.7 (6) | C53—C54—C55—C56 | 0.0 |
N9—Ni3—N12—C70 | 95.4 (7) | C59—C54—C55—C56 | −179.3 (10) |
Cl4—Ni3—N12—C70 | −173.4 (6) | C54—C55—C56—C57 | 0.0 |
Cl3—Ni3—N12—C70 | −82.4 (6) | C55—C56—C57—C62 | 179.6 (10) |
C9—N1—C1—C2 | 2.9 (12) | C55—C56—C57—C58 | 0.0 |
Ni1—N1—C1—C2 | 177.9 (4) | C64—N10—C58—C57 | −1.3 (12) |
C9—N1—C1—C6 | 178.4 (8) | Ni3—N10—C58—C57 | 179.8 (3) |
Ni1—N1—C1—C6 | −6.7 (8) | C64—N10—C58—C53 | −177.3 (8) |
N1—C1—C2—C7 | −5.1 (9) | Ni3—N10—C58—C53 | 3.8 (8) |
C6—C1—C2—C7 | 179.5 (9) | C62—C57—C58—N10 | 4.6 (9) |
N1—C1—C2—C3 | 175.4 (7) | C56—C57—C58—N10 | −175.8 (7) |
C6—C1—C2—C3 | 0.0 | C62—C57—C58—C53 | −179.6 (9) |
C7—C2—C3—C4 | −179.5 (10) | C56—C57—C58—C53 | 0.0 |
C1—C2—C3—C4 | 0.0 | N9—C53—C58—N10 | −6.3 (9) |
C2—C3—C4—C5 | 0.0 | C54—C53—C58—N10 | 176.0 (7) |
C3—C4—C5—C10 | −179.2 (10) | N9—C53—C58—C57 | 177.6 (7) |
C3—C4—C5—C6 | 0.0 | C54—C53—C58—C57 | 0.0 |
C12—N2—C6—C5 | 2.6 (12) | C55—C54—C59—C60 | 177.4 (10) |
Ni1—N2—C6—C5 | 179.3 (3) | C53—C54—C59—C60 | −1.9 (16) |
C12—N2—C6—C1 | −179.7 (8) | C54—C59—C60—C61 | 0 (2) |
Ni1—N2—C6—C1 | −3.0 (8) | C53—N9—C61—C60 | −1.5 (18) |
C10—C5—C6—N2 | −3.1 (9) | Ni3—N9—C61—C60 | 174.8 (9) |
C4—C5—C6—N2 | 177.6 (7) | C59—C60—C61—N9 | 1 (2) |
C10—C5—C6—C1 | 179.3 (9) | C56—C57—C62—C63 | 175.7 (8) |
C4—C5—C6—C1 | 0.0 | C58—C57—C62—C63 | −4.7 (14) |
N1—C1—C6—N2 | 6.7 (9) | C57—C62—C63—C64 | 1.9 (18) |
C2—C1—C6—N2 | −177.7 (7) | C58—N10—C64—C63 | −1.7 (18) |
N1—C1—C6—C5 | −175.5 (7) | Ni3—N10—C64—C63 | 177.0 (8) |
C2—C1—C6—C5 | 0.0 | C62—C63—C64—N10 | 1.4 (19) |
C1—C2—C7—C8 | 3.8 (15) | C73—N11—C65—C66 | −3.5 (12) |
C3—C2—C7—C8 | −176.7 (9) | Ni3—N11—C65—C66 | −178.0 (4) |
C2—C7—C8—C9 | −0.5 (18) | C73—N11—C65—C70 | 178.9 (8) |
C1—N1—C9—C8 | 0.6 (18) | Ni3—N11—C65—C70 | 4.4 (8) |
Ni1—N1—C9—C8 | −173.3 (8) | N11—C65—C66—C67 | −177.6 (8) |
C7—C8—C9—N1 | −1.8 (19) | C70—C65—C66—C67 | 0.0 |
C6—C5—C10—C11 | 1.2 (15) | N11—C65—C66—C71 | 5.9 (9) |
C4—C5—C10—C11 | −179.6 (9) | C70—C65—C66—C71 | −176.5 (8) |
C5—C10—C11—C12 | 1.2 (19) | C65—C66—C67—C68 | 0.0 |
C6—N2—C12—C11 | 0.0 (17) | C71—C66—C67—C68 | 176.3 (8) |
Ni1—N2—C12—C11 | −176.3 (7) | C66—C67—C68—C69 | 0.0 |
C10—C11—C12—N2 | −1.8 (18) | C67—C68—C69—C70 | 0.0 |
C21—N3—C13—C14 | 4.2 (12) | C67—C68—C69—C74 | 179.4 (8) |
Ni1—N3—C13—C14 | 177.9 (4) | C76—N12—C70—C69 | −1.8 (12) |
C21—N3—C13—C18 | −178.0 (8) | Ni3—N12—C70—C69 | 178.9 (4) |
Ni1—N3—C13—C18 | −4.2 (8) | C76—N12—C70—C65 | 178.1 (8) |
N3—C13—C14—C15 | 177.8 (8) | Ni3—N12—C70—C65 | −1.2 (8) |
C18—C13—C14—C15 | 0.0 | C68—C69—C70—N12 | 179.9 (8) |
N3—C13—C14—C19 | −3.4 (9) | C74—C69—C70—N12 | 0.5 (9) |
C18—C13—C14—C19 | 178.8 (8) | C68—C69—C70—C65 | 0.0 |
C13—C14—C15—C16 | 0.0 | C74—C69—C70—C65 | −179.4 (8) |
C19—C14—C15—C16 | −178.7 (8) | N11—C65—C70—N12 | −2.2 (9) |
C14—C15—C16—C17 | 0.0 | C66—C65—C70—N12 | −179.9 (8) |
C15—C16—C17—C18 | 0.0 | N11—C65—C70—C69 | 177.7 (8) |
C15—C16—C17—C22 | 180.0 (9) | C66—C65—C70—C69 | 0.0 |
C24—N4—C18—C17 | −0.2 (12) | C65—C66—C71—C72 | −4.0 (14) |
Ni1—N4—C18—C17 | −178.7 (4) | C67—C66—C71—C72 | 179.6 (9) |
C24—N4—C18—C13 | −179.8 (8) | C66—C71—C72—C73 | −0.2 (18) |
Ni1—N4—C18—C13 | 1.8 (8) | C65—N11—C73—C72 | −1.1 (16) |
C16—C17—C18—N4 | −179.6 (8) | Ni3—N11—C73—C72 | 172.4 (9) |
C22—C17—C18—N4 | 0.4 (9) | C71—C72—C73—N11 | 2.8 (18) |
C16—C17—C18—C13 | 0.0 | C68—C69—C74—C75 | 179.7 (9) |
C22—C17—C18—C13 | 180.0 (8) | C70—C69—C74—C75 | −0.9 (14) |
N3—C13—C18—N4 | 1.7 (9) | C69—C74—C75—C76 | 2.6 (19) |
C14—C13—C18—N4 | 179.6 (8) | C70—N12—C76—C75 | 3.5 (18) |
N3—C13—C18—C17 | −177.9 (8) | Ni3—N12—C76—C75 | −177.2 (9) |
C14—C13—C18—C17 | 0.0 | C74—C75—C76—N12 | −4 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···Cl3 | 0.82 | 2.50 | 3.185 (8) | 142 |
O1W—H1W2···Cl5 | 0.82 | 2.41 | 3.095 (10) | 141 |
O2W—H2W1···Cl1 | 0.82 | 2.36 | 3.182 (8) | 180 |
O2W—H2W2···Cl6 | 0.82 | 2.31 | 3.123 (10) | 172 |
Experimental details
Crystal data | |
Chemical formula | [Ni(C14H16N2)2(H2O)2]Cl2·2[NiCl2(C12H8N2)2] |
Mr | 1570.25 |
Crystal system, space group | Monoclinic, P21 |
Temperature (K) | 293 |
a, b, c (Å) | 12.390 (2), 13.819 (2), 21.261 (3) |
β (°) | 101.348 (2) |
V (Å3) | 3569.1 (9) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 1.06 |
Crystal size (mm) | 0.48 × 0.23 × 0.18 |
Data collection | |
Diffractometer | Bruker APEX area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.629, 0.832 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 22161, 14184, 7201 |
Rint | 0.046 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.056, 0.165, 1.02 |
No. of reflections | 14184 |
No. of parameters | 796 |
No. of restraints | 590 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.73, −0.50 |
Absolute structure | Flack (1983), 5767 Friedel pairs |
Absolute structure parameter | −0.07 (3) |
Computer programs: SMART (Bruker, 2003), SAINT (Bruker, 2003), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···Cl3 | 0.82 | 2.50 | 3.185 (8) | 142 |
O1W—H1W2···Cl5 | 0.82 | 2.41 | 3.095 (10) | 141 |
O2W—H2W1···Cl1 | 0.82 | 2.36 | 3.182 (8) | 180 |
O2W—H2W2···Cl6 | 0.82 | 2.31 | 3.123 (10) | 172 |
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1,2-Diphenylethylenediamine, which can exist in the meso and the optically active R,R and S,S forms, behaves like ethylenediamine in a number of metal complexes; several nickel(II) complexes have been characterized by crystallography. These have the ligand functioning in the expected chelating mode, as noted in the nitrite/perchlorate, nitrite/chloride (Finney et al., 1981), dichloride (García-Granda & Gómez-Beltrán, 1984; Murmann & Barnes, 2004) and acetate (García-Granda et al., 1990) derivatives. The dichloride complexes are ionic and there is no direct interaction between the four-coordinate cation and the halide.
The attempt to synthesize a similar, mixed-ligand complex, by adding a molar equivalent of 1,10-phenanthroline yielded a cocrystal of dichlorobis(phenanthroline)nickel and diaquabis(diphenylethylenediamine)nickel dichloride (Fig. 1). The trinuclear compound lies on a false inversion site. The nickel atom of the diaquabis(diphenylethylenediamine)nickel cation lies on this site, which also relates the two neutral dichlorobis(phenanthroline)nickel to each other. The cation uses its water molecules to form hydrogen bonds to the free chlorine anion as well as to the chlorine atom of the neutral molecule. The three nickel atoms exist in octahedral geometries.