Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806013250/kp2015sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806013250/kp2015Isup2.hkl |
CCDC reference: 608438
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.006 Å Some non-H atoms missing
- R factor = 0.045
- wR factor = 0.128
- Data-to-parameter ratio = 16.1
checkCIF/PLATON results
No syntax errors found
Alert level A ABSMU01_ALERT_1_A The ratio of given/expected absorption coefficient lies outside the range 0.90 <> 1.10 Calculated value of mu = 3.249 Value of mu given = 1.624 CHEMW03_ALERT_2_A ALERT: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 711.76 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 14.00 168.15 H 1.01 14.00 14.11 N 14.01 2.00 28.01 O 16.00 1.00 16.00 Cl 35.45 2.00 70.91 Ni 58.69 1.00 58.69 Calculated formula weight 355.88 DENSD01_ALERT_1_A The ratio of the submitted crystal density and that calculated from the formula is outside the range 0.90 <> 1.10 Crystal density given = 1.556 Calculated crystal density = 3.113 PLAT043_ALERT_1_A Check Reported Molecular Weight ................ 711.76 PLAT046_ALERT_1_A Reported Z, MW and D(calc) are Inconsistent .... 3.11
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.13 PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C1 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C14 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C28 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C14 H14 Cl2 N2 Ni O
Alert level G FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data. Atom count from _chemical_formula_sum:C28 H28 Cl4 N4 Ni2 O2 Atom count from the _atom_site data: C14 H14 Cl2 N2 Ni1 O1 CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected. CELLZ01_ALERT_1_G ALERT: Large difference may be due to a symmetry error - see SYMMG tests From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_sum C28 H28 Cl4 N4 Ni2 O2 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 112.00 56.00 56.00 H 112.00 56.00 56.00 Cl 16.00 8.00 8.00 N 16.00 8.00 8.00 Ni 8.00 4.00 4.00 O 8.00 4.00 4.00
5 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 10 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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 6 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 2003).
[NiCl2(C14H12N2)(H2O)] | Z = 4 |
Mr = 711.76 | F(000) = 728 |
Triclinic, P1 | Dx = 1.556 Mg m−3 |
a = 7.5631 (13) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 11.501 (2) Å | Cell parameters from 3906 reflections |
c = 18.924 (4) Å | θ = 2.5–26.0° |
α = 106.692 (3)° | µ = 1.62 mm−1 |
β = 93.545 (4)° | T = 293 K |
γ = 103.467 (2)° | Plate, green |
V = 1518.7 (5) Å3 | 0.30 × 0.16 × 0.06 mm |
Siemens SMART 1000 CCD area-detector diffractometer | 5826 independent reflections |
Radiation source: fine-focus sealed tube | 4892 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.017 |
Detector resolution: 8.33 pixels mm-1 | θmax = 26.1°, θmin = 1.9° |
ω scans | h = −9→9 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −13→14 |
Tmin = 0.641, Tmax = 0.909 | l = −22→23 |
8714 measured reflections |
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)] = 0.045 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.128 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0726P)2 + 0.9988P] where P = (Fo2 + 2Fc2)/3 |
5826 reflections | (Δ/σ)max = 0.001 |
361 parameters | Δρmax = 1.04 e Å−3 |
0 restraints | Δρmin = −0.49 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 | ||
Ni1 | 1.58716 (6) | 0.67800 (4) | 0.34192 (2) | 0.03713 (14) | |
Ni2 | 0.94287 (6) | 0.33724 (4) | 0.15800 (2) | 0.03489 (14) | |
Cl1 | 1.37032 (13) | 0.73474 (8) | 0.27395 (5) | 0.0477 (2) | |
Cl2 | 1.86982 (12) | 0.64222 (8) | 0.37593 (5) | 0.0446 (2) | |
Cl3 | 0.70694 (14) | 0.29197 (8) | 0.22906 (5) | 0.0496 (2) | |
Cl4 | 1.23711 (12) | 0.38200 (8) | 0.12324 (5) | 0.0446 (2) | |
O1 | 1.5603 (4) | 0.5290 (3) | 0.25056 (16) | 0.0637 (8) | |
O2 | 1.0076 (4) | 0.5155 (2) | 0.22627 (16) | 0.0570 (7) | |
N1 | 1.6698 (4) | 0.8525 (3) | 0.42006 (16) | 0.0376 (6) | |
N2 | 1.4477 (4) | 0.6378 (3) | 0.42570 (15) | 0.0368 (6) | |
N3 | 0.8010 (4) | 0.3136 (3) | 0.05664 (16) | 0.0411 (7) | |
N4 | 0.9095 (4) | 0.1476 (3) | 0.11276 (15) | 0.0370 (6) | |
C1 | 1.8331 (6) | 0.9566 (4) | 0.3401 (2) | 0.0606 (11) | |
H1B | 1.7823 | 0.8743 | 0.3051 | 0.091* | |
H1C | 1.9646 | 0.9770 | 0.3442 | 0.091* | |
H1D | 1.7894 | 1.0173 | 0.3231 | 0.091* | |
C2 | 1.7756 (5) | 0.9587 (3) | 0.4143 (2) | 0.0435 (8) | |
C3 | 1.8302 (5) | 1.0684 (3) | 0.4768 (2) | 0.0491 (9) | |
H3A | 1.9020 | 1.1423 | 0.4717 | 0.059* | |
C4 | 1.7786 (5) | 1.0673 (3) | 0.5446 (2) | 0.0483 (9) | |
H4A | 1.8154 | 1.1396 | 0.5855 | 0.058* | |
C5 | 1.6693 (5) | 0.9553 (3) | 0.5517 (2) | 0.0420 (8) | |
C6 | 1.6092 (6) | 0.9443 (4) | 0.6204 (2) | 0.0506 (9) | |
H6A | 1.6465 | 1.0129 | 0.6635 | 0.061* | |
C7 | 1.4989 (6) | 0.8353 (4) | 0.6231 (2) | 0.0535 (10) | |
H7A | 1.4623 | 0.8298 | 0.6683 | 0.064* | |
C8 | 1.4376 (5) | 0.7288 (4) | 0.5583 (2) | 0.0452 (8) | |
C9 | 1.3164 (6) | 0.6160 (4) | 0.5575 (2) | 0.0534 (10) | |
H9A | 1.2736 | 0.6067 | 0.6011 | 0.064* | |
C10 | 1.2616 (6) | 0.5202 (4) | 0.4924 (2) | 0.0536 (10) | |
H10A | 1.1786 | 0.4460 | 0.4917 | 0.064* | |
C11 | 1.3282 (5) | 0.5311 (3) | 0.4261 (2) | 0.0448 (8) | |
C12 | 1.4990 (5) | 0.7351 (3) | 0.49064 (18) | 0.0356 (7) | |
C13 | 1.6168 (5) | 0.8503 (3) | 0.48725 (19) | 0.0362 (7) | |
C14 | 1.2658 (7) | 0.4242 (4) | 0.3551 (2) | 0.0641 (12) | |
H14A | 1.3234 | 0.4475 | 0.3155 | 0.096* | |
H14B | 1.1349 | 0.4051 | 0.3432 | 0.096* | |
H14C | 1.2991 | 0.3516 | 0.3609 | 0.096* | |
C15 | 0.8093 (8) | 0.5331 (4) | 0.0754 (3) | 0.0771 (15) | |
H15A | 0.8719 | 0.5414 | 0.1231 | 0.116* | |
H15B | 0.7011 | 0.5628 | 0.0823 | 0.116* | |
H15C | 0.8891 | 0.5819 | 0.0509 | 0.116* | |
C16 | 0.7561 (5) | 0.3977 (4) | 0.0288 (2) | 0.0523 (10) | |
C17 | 0.6596 (6) | 0.3603 (5) | −0.0446 (3) | 0.0660 (12) | |
H17A | 0.6292 | 0.4201 | −0.0638 | 0.079* | |
C18 | 0.6123 (6) | 0.2378 (5) | −0.0863 (2) | 0.0668 (12) | |
H18A | 0.5497 | 0.2139 | −0.1342 | 0.080* | |
C19 | 0.6558 (5) | 0.1468 (4) | −0.0584 (2) | 0.0529 (10) | |
C20 | 0.6061 (6) | 0.0135 (5) | −0.0978 (2) | 0.0614 (12) | |
H20A | 0.5401 | −0.0154 | −0.1454 | 0.074* | |
C21 | 0.6515 (6) | −0.0698 (4) | −0.0683 (2) | 0.0566 (11) | |
H21A | 0.6149 | −0.1550 | −0.0950 | 0.068* | |
C22 | 0.7564 (5) | −0.0286 (4) | 0.0042 (2) | 0.0458 (9) | |
C23 | 0.8121 (6) | −0.1090 (3) | 0.0390 (2) | 0.0529 (10) | |
H23A | 0.7802 | −0.1953 | 0.0150 | 0.063* | |
C24 | 0.9129 (6) | −0.0611 (3) | 0.1077 (2) | 0.0514 (10) | |
H24A | 0.9487 | −0.1148 | 0.1308 | 0.062* | |
C25 | 0.9631 (5) | 0.0692 (3) | 0.1440 (2) | 0.0431 (8) | |
C26 | 0.8079 (5) | 0.1011 (3) | 0.04438 (19) | 0.0390 (8) | |
C27 | 0.7537 (5) | 0.1897 (3) | 0.01369 (19) | 0.0419 (8) | |
C28 | 1.0790 (6) | 0.1253 (4) | 0.2183 (2) | 0.0564 (10) | |
H28A | 1.0984 | 0.2150 | 0.2340 | 0.085* | |
H28B | 1.1951 | 0.1053 | 0.2149 | 0.085* | |
H28C | 1.0180 | 0.0917 | 0.2540 | 0.085* | |
H1W1 | 1.5539 | 0.4525 | 0.2266 | 0.068* | |
H2W1 | 1.5323 | 0.5635 | 0.2185 | 0.068* | |
H1W2 | 1.0953 | 0.5784 | 0.2272 | 0.068* | |
H2W2 | 0.9638 | 0.5366 | 0.2675 | 0.068* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0402 (3) | 0.0310 (2) | 0.0333 (2) | 0.00561 (18) | 0.00384 (18) | 0.00275 (18) |
Ni2 | 0.0405 (3) | 0.0273 (2) | 0.0317 (2) | 0.00618 (18) | 0.00371 (18) | 0.00366 (17) |
Cl1 | 0.0548 (6) | 0.0366 (5) | 0.0443 (5) | 0.0086 (4) | −0.0039 (4) | 0.0064 (4) |
Cl2 | 0.0396 (5) | 0.0396 (5) | 0.0465 (5) | 0.0075 (4) | 0.0037 (4) | 0.0035 (4) |
Cl3 | 0.0563 (6) | 0.0395 (5) | 0.0479 (5) | 0.0095 (4) | 0.0198 (4) | 0.0056 (4) |
Cl4 | 0.0416 (5) | 0.0362 (4) | 0.0458 (5) | 0.0047 (4) | 0.0066 (4) | 0.0013 (4) |
O1 | 0.072 (2) | 0.0508 (17) | 0.0518 (17) | 0.0284 (15) | −0.0143 (15) | −0.0140 (13) |
O2 | 0.0560 (17) | 0.0355 (14) | 0.0594 (17) | −0.0008 (12) | 0.0181 (14) | −0.0079 (12) |
N1 | 0.0374 (16) | 0.0313 (14) | 0.0394 (16) | 0.0058 (12) | 0.0023 (12) | 0.0074 (12) |
N2 | 0.0399 (16) | 0.0312 (14) | 0.0363 (15) | 0.0075 (12) | −0.0001 (12) | 0.0084 (12) |
N3 | 0.0379 (16) | 0.0439 (17) | 0.0391 (16) | 0.0046 (13) | 0.0069 (13) | 0.0141 (13) |
N4 | 0.0402 (16) | 0.0315 (14) | 0.0329 (15) | 0.0037 (12) | 0.0098 (12) | 0.0041 (12) |
C1 | 0.061 (3) | 0.054 (2) | 0.063 (3) | 0.001 (2) | 0.012 (2) | 0.024 (2) |
C2 | 0.0371 (19) | 0.0373 (19) | 0.054 (2) | 0.0057 (15) | 0.0024 (16) | 0.0146 (17) |
C3 | 0.042 (2) | 0.0308 (18) | 0.066 (3) | 0.0009 (15) | −0.0040 (18) | 0.0112 (17) |
C4 | 0.044 (2) | 0.0329 (19) | 0.055 (2) | 0.0079 (16) | −0.0061 (17) | −0.0011 (17) |
C5 | 0.043 (2) | 0.0315 (18) | 0.047 (2) | 0.0127 (15) | −0.0031 (16) | 0.0035 (15) |
C6 | 0.064 (3) | 0.043 (2) | 0.038 (2) | 0.0202 (19) | −0.0025 (18) | −0.0003 (16) |
C7 | 0.072 (3) | 0.055 (2) | 0.036 (2) | 0.024 (2) | 0.0118 (19) | 0.0106 (18) |
C8 | 0.050 (2) | 0.043 (2) | 0.044 (2) | 0.0163 (17) | 0.0054 (17) | 0.0131 (16) |
C9 | 0.058 (2) | 0.056 (2) | 0.051 (2) | 0.012 (2) | 0.0156 (19) | 0.026 (2) |
C10 | 0.053 (2) | 0.046 (2) | 0.060 (3) | −0.0003 (18) | 0.0040 (19) | 0.024 (2) |
C11 | 0.045 (2) | 0.0357 (19) | 0.050 (2) | 0.0033 (15) | −0.0029 (16) | 0.0158 (16) |
C12 | 0.0391 (18) | 0.0298 (16) | 0.0361 (17) | 0.0110 (14) | 0.0009 (14) | 0.0070 (14) |
C13 | 0.0355 (18) | 0.0313 (17) | 0.0377 (18) | 0.0095 (14) | 0.0000 (14) | 0.0047 (14) |
C14 | 0.076 (3) | 0.040 (2) | 0.057 (3) | −0.010 (2) | −0.011 (2) | 0.0098 (19) |
C15 | 0.084 (4) | 0.058 (3) | 0.099 (4) | 0.021 (3) | 0.002 (3) | 0.040 (3) |
C16 | 0.043 (2) | 0.056 (2) | 0.062 (3) | 0.0071 (18) | 0.0057 (18) | 0.030 (2) |
C17 | 0.058 (3) | 0.081 (3) | 0.073 (3) | 0.014 (2) | 0.005 (2) | 0.050 (3) |
C18 | 0.054 (3) | 0.094 (4) | 0.046 (2) | 0.006 (2) | 0.003 (2) | 0.024 (2) |
C19 | 0.039 (2) | 0.072 (3) | 0.043 (2) | 0.0059 (19) | 0.0099 (17) | 0.019 (2) |
C20 | 0.042 (2) | 0.080 (3) | 0.037 (2) | 0.002 (2) | 0.0003 (17) | −0.009 (2) |
C21 | 0.041 (2) | 0.054 (2) | 0.051 (2) | −0.0009 (18) | 0.0064 (18) | −0.009 (2) |
C22 | 0.0330 (18) | 0.043 (2) | 0.044 (2) | −0.0023 (15) | 0.0138 (15) | −0.0044 (16) |
C23 | 0.051 (2) | 0.0294 (18) | 0.066 (3) | 0.0019 (16) | 0.023 (2) | 0.0002 (18) |
C24 | 0.055 (2) | 0.037 (2) | 0.063 (3) | 0.0119 (17) | 0.023 (2) | 0.0146 (18) |
C25 | 0.050 (2) | 0.0349 (18) | 0.046 (2) | 0.0108 (16) | 0.0188 (17) | 0.0123 (16) |
C26 | 0.0351 (18) | 0.0404 (19) | 0.0345 (18) | 0.0052 (14) | 0.0117 (14) | 0.0033 (15) |
C27 | 0.0346 (18) | 0.049 (2) | 0.0338 (18) | 0.0020 (15) | 0.0099 (14) | 0.0069 (16) |
C28 | 0.077 (3) | 0.055 (2) | 0.044 (2) | 0.023 (2) | 0.009 (2) | 0.0197 (19) |
Ni1—O1 | 2.015 (3) | C8—C9 | 1.399 (5) |
Ni1—N1 | 2.049 (3) | C8—C12 | 1.403 (5) |
Ni1—N2 | 2.059 (3) | C9—C10 | 1.360 (6) |
Ni1—Cl1 | 2.3431 (10) | C9—H9A | 0.9300 |
Ni1—Cl2 | 2.3548 (10) | C10—C11 | 1.408 (6) |
Ni2—O2 | 2.011 (3) | C10—H10A | 0.9300 |
Ni2—N4 | 2.049 (3) | C11—C14 | 1.498 (5) |
Ni2—N3 | 2.053 (3) | C12—C13 | 1.435 (5) |
Ni2—Cl4 | 2.3435 (10) | C14—H14A | 0.9600 |
Ni2—Cl3 | 2.3515 (10) | C14—H14B | 0.9600 |
O1—H1W1 | 0.8541 | C14—H14C | 0.9600 |
O1—H2W1 | 0.8560 | C15—C16 | 1.497 (6) |
O2—H1W2 | 0.8552 | C15—H15A | 0.9600 |
O2—H2W2 | 0.8599 | C15—H15B | 0.9600 |
N1—C2 | 1.333 (4) | C15—H15C | 0.9600 |
N1—C13 | 1.362 (4) | C16—C17 | 1.426 (6) |
N2—C11 | 1.347 (4) | C17—C18 | 1.352 (7) |
N2—C12 | 1.364 (4) | C17—H17A | 0.9300 |
N3—C16 | 1.324 (5) | C18—C19 | 1.392 (6) |
N3—C27 | 1.371 (5) | C18—H18A | 0.9300 |
N4—C25 | 1.332 (5) | C19—C27 | 1.404 (5) |
N4—C26 | 1.356 (4) | C19—C20 | 1.445 (6) |
C1—C2 | 1.492 (6) | C20—C21 | 1.335 (7) |
C1—H1B | 0.9600 | C20—H20A | 0.9300 |
C1—H1C | 0.9600 | C21—C22 | 1.433 (6) |
C1—H1D | 0.9600 | C21—H21A | 0.9300 |
C2—C3 | 1.415 (5) | C22—C23 | 1.402 (6) |
C3—C4 | 1.365 (6) | C22—C26 | 1.413 (5) |
C3—H3A | 0.9300 | C23—C24 | 1.359 (6) |
C4—C5 | 1.407 (5) | C23—H23A | 0.9300 |
C4—H4A | 0.9300 | C24—C25 | 1.405 (5) |
C5—C13 | 1.405 (5) | C24—H24A | 0.9300 |
C5—C6 | 1.432 (5) | C25—C28 | 1.492 (5) |
C6—C7 | 1.352 (6) | C26—C27 | 1.432 (5) |
C6—H6A | 0.9300 | C28—H28A | 0.9600 |
C7—C8 | 1.422 (5) | C28—H28B | 0.9600 |
C7—H7A | 0.9300 | C28—H28C | 0.9600 |
O1—Ni1—N1 | 163.92 (13) | C8—C9—H9A | 120.3 |
O1—Ni1—N2 | 114.49 (13) | C9—C10—C11 | 121.2 (4) |
N1—Ni1—N2 | 81.34 (11) | C9—C10—H10A | 119.4 |
O1—Ni1—Cl1 | 86.19 (8) | C11—C10—H10A | 119.4 |
N1—Ni1—Cl1 | 93.37 (8) | N2—C11—C10 | 120.5 (3) |
N2—Ni1—Cl1 | 102.18 (8) | N2—C11—C14 | 119.2 (3) |
O1—Ni1—Cl2 | 85.87 (8) | C10—C11—C14 | 120.3 (3) |
N1—Ni1—Cl2 | 88.73 (8) | N2—C12—C8 | 123.5 (3) |
N2—Ni1—Cl2 | 99.63 (8) | N2—C12—C13 | 116.8 (3) |
Cl1—Ni1—Cl2 | 158.16 (4) | C8—C12—C13 | 119.6 (3) |
O2—Ni2—N4 | 164.58 (12) | N1—C13—C5 | 123.1 (3) |
O2—Ni2—N3 | 113.46 (13) | N1—C13—C12 | 117.4 (3) |
N4—Ni2—N3 | 81.94 (12) | C5—C13—C12 | 119.5 (3) |
O2—Ni2—Cl4 | 87.41 (8) | C11—C14—H14A | 109.5 |
N4—Ni2—Cl4 | 91.66 (8) | C11—C14—H14B | 109.5 |
N3—Ni2—Cl4 | 96.50 (8) | H14A—C14—H14B | 109.5 |
O2—Ni2—Cl3 | 87.44 (8) | C11—C14—H14C | 109.5 |
N4—Ni2—Cl3 | 88.35 (8) | H14A—C14—H14C | 109.5 |
N3—Ni2—Cl3 | 102.81 (9) | H14B—C14—H14C | 109.5 |
Cl4—Ni2—Cl3 | 160.50 (4) | C16—C15—H15A | 109.5 |
Ni1—O1—H1W1 | 155.8 | C16—C15—H15B | 109.5 |
Ni1—O1—H2W1 | 97.2 | H15A—C15—H15B | 109.5 |
H1W1—O1—H2W1 | 106.8 | C16—C15—H15C | 109.5 |
Ni2—O2—H1W2 | 129.8 | H15A—C15—H15C | 109.5 |
Ni2—O2—H2W2 | 122.5 | H15B—C15—H15C | 109.5 |
H1W2—O2—H2W2 | 106.3 | N3—C16—C17 | 120.7 (4) |
C2—N1—C13 | 119.1 (3) | N3—C16—C15 | 118.9 (4) |
C2—N1—Ni1 | 128.9 (3) | C17—C16—C15 | 120.4 (4) |
C13—N1—Ni1 | 111.8 (2) | C18—C17—C16 | 119.9 (4) |
C11—N2—C12 | 118.2 (3) | C18—C17—H17A | 120.1 |
C11—N2—Ni1 | 130.0 (2) | C16—C17—H17A | 120.1 |
C12—N2—Ni1 | 111.6 (2) | C17—C18—C19 | 120.9 (4) |
C16—N3—C27 | 119.0 (3) | C17—C18—H18A | 119.5 |
C16—N3—Ni2 | 130.1 (3) | C19—C18—H18A | 119.5 |
C27—N3—Ni2 | 111.0 (2) | C18—C19—C27 | 116.5 (4) |
C25—N4—C26 | 119.5 (3) | C18—C19—C20 | 124.9 (4) |
C25—N4—Ni2 | 128.3 (2) | C27—C19—C20 | 118.6 (4) |
C26—N4—Ni2 | 112.1 (2) | C21—C20—C19 | 122.3 (4) |
C2—C1—H1B | 109.5 | C21—C20—H20A | 118.8 |
C2—C1—H1C | 109.5 | C19—C20—H20A | 118.8 |
H1B—C1—H1C | 109.5 | C20—C21—C22 | 120.4 (4) |
C2—C1—H1D | 109.5 | C20—C21—H21A | 119.8 |
H1B—C1—H1D | 109.5 | C22—C21—H21A | 119.8 |
H1C—C1—H1D | 109.5 | C23—C22—C26 | 116.8 (4) |
N1—C2—C3 | 120.6 (3) | C23—C22—C21 | 124.3 (4) |
N1—C2—C1 | 117.5 (3) | C26—C22—C21 | 118.9 (4) |
C3—C2—C1 | 121.9 (3) | C24—C23—C22 | 120.1 (3) |
C4—C3—C2 | 120.8 (3) | C24—C23—H23A | 120.0 |
C4—C3—H3A | 119.6 | C22—C23—H23A | 120.0 |
C2—C3—H3A | 119.6 | C23—C24—C25 | 120.3 (4) |
C3—C4—C5 | 119.2 (3) | C23—C24—H24A | 119.9 |
C3—C4—H4A | 120.4 | C25—C24—H24A | 119.9 |
C5—C4—H4A | 120.4 | N4—C25—C24 | 120.9 (4) |
C13—C5—C4 | 117.2 (4) | N4—C25—C28 | 117.4 (3) |
C13—C5—C6 | 119.4 (3) | C24—C25—C28 | 121.7 (4) |
C4—C5—C6 | 123.4 (3) | N4—C26—C22 | 122.4 (3) |
C7—C6—C5 | 120.6 (3) | N4—C26—C27 | 117.0 (3) |
C7—C6—H6A | 119.7 | C22—C26—C27 | 120.5 (3) |
C5—C6—H6A | 119.7 | N3—C27—C19 | 123.0 (4) |
C6—C7—C8 | 121.3 (4) | N3—C27—C26 | 117.9 (3) |
C6—C7—H7A | 119.3 | C19—C27—C26 | 119.1 (3) |
C8—C7—H7A | 119.3 | C25—C28—H28A | 109.5 |
C9—C8—C12 | 117.1 (3) | C25—C28—H28B | 109.5 |
C9—C8—C7 | 123.5 (4) | H28A—C28—H28B | 109.5 |
C12—C8—C7 | 119.4 (4) | C25—C28—H28C | 109.5 |
C10—C9—C8 | 119.4 (4) | H28A—C28—H28C | 109.5 |
C10—C9—H9A | 120.3 | H28B—C28—H28C | 109.5 |
O1—Ni1—N1—C2 | 12.5 (6) | C9—C8—C12—N2 | −0.4 (5) |
N2—Ni1—N1—C2 | −177.3 (3) | C7—C8—C12—N2 | −180.0 (3) |
Cl1—Ni1—N1—C2 | −75.5 (3) | C9—C8—C12—C13 | 177.1 (3) |
Cl2—Ni1—N1—C2 | 82.8 (3) | C7—C8—C12—C13 | −2.4 (5) |
O1—Ni1—N1—C13 | −161.8 (3) | C2—N1—C13—C5 | −0.3 (5) |
N2—Ni1—N1—C13 | 8.4 (2) | Ni1—N1—C13—C5 | 174.6 (3) |
Cl1—Ni1—N1—C13 | 110.3 (2) | C2—N1—C13—C12 | 178.4 (3) |
Cl2—Ni1—N1—C13 | −91.5 (2) | Ni1—N1—C13—C12 | −6.7 (4) |
O1—Ni1—N2—C11 | −7.2 (3) | C4—C5—C13—N1 | 1.3 (5) |
N1—Ni1—N2—C11 | 175.8 (3) | C6—C5—C13—N1 | −179.2 (3) |
Cl1—Ni1—N2—C11 | 84.2 (3) | C4—C5—C13—C12 | −177.4 (3) |
Cl2—Ni1—N2—C11 | −97.0 (3) | C6—C5—C13—C12 | 2.1 (5) |
O1—Ni1—N2—C12 | 168.1 (2) | N2—C12—C13—N1 | −1.0 (4) |
N1—Ni1—N2—C12 | −9.0 (2) | C8—C12—C13—N1 | −178.7 (3) |
Cl1—Ni1—N2—C12 | −100.6 (2) | N2—C12—C13—C5 | 177.8 (3) |
Cl2—Ni1—N2—C12 | 78.2 (2) | C8—C12—C13—C5 | 0.1 (5) |
O2—Ni2—N3—C16 | 4.2 (4) | C27—N3—C16—C17 | 0.2 (5) |
N4—Ni2—N3—C16 | −176.5 (3) | Ni2—N3—C16—C17 | 178.5 (3) |
Cl4—Ni2—N3—C16 | −85.7 (3) | C27—N3—C16—C15 | −179.4 (4) |
Cl3—Ni2—N3—C16 | 97.0 (3) | Ni2—N3—C16—C15 | −1.2 (6) |
O2—Ni2—N3—C27 | −177.4 (2) | N3—C16—C17—C18 | 0.3 (6) |
N4—Ni2—N3—C27 | 1.8 (2) | C15—C16—C17—C18 | 180.0 (4) |
Cl4—Ni2—N3—C27 | 92.6 (2) | C16—C17—C18—C19 | 0.3 (7) |
Cl3—Ni2—N3—C27 | −84.6 (2) | C17—C18—C19—C27 | −1.4 (6) |
O2—Ni2—N4—C25 | −1.0 (6) | C17—C18—C19—C20 | 178.0 (4) |
N3—Ni2—N4—C25 | −178.4 (3) | C18—C19—C20—C21 | −180.0 (4) |
Cl4—Ni2—N4—C25 | 85.3 (3) | C27—C19—C20—C21 | −0.6 (6) |
Cl3—Ni2—N4—C25 | −75.2 (3) | C19—C20—C21—C22 | −1.3 (6) |
O2—Ni2—N4—C26 | 174.1 (4) | C20—C21—C22—C23 | −179.2 (4) |
N3—Ni2—N4—C26 | −3.3 (2) | C20—C21—C22—C26 | 1.2 (6) |
Cl4—Ni2—N4—C26 | −99.6 (2) | C26—C22—C23—C24 | −0.9 (5) |
Cl3—Ni2—N4—C26 | 99.9 (2) | C21—C22—C23—C24 | 179.5 (4) |
C13—N1—C2—C3 | −0.9 (5) | C22—C23—C24—C25 | −0.6 (6) |
Ni1—N1—C2—C3 | −174.9 (3) | C26—N4—C25—C24 | −1.2 (5) |
C13—N1—C2—C1 | 179.0 (3) | Ni2—N4—C25—C24 | 173.5 (3) |
Ni1—N1—C2—C1 | 5.1 (5) | C26—N4—C25—C28 | 178.3 (3) |
N1—C2—C3—C4 | 1.3 (6) | Ni2—N4—C25—C28 | −7.0 (5) |
C1—C2—C3—C4 | −178.7 (4) | C23—C24—C25—N4 | 1.6 (6) |
C2—C3—C4—C5 | −0.3 (6) | C23—C24—C25—C28 | −177.8 (4) |
C3—C4—C5—C13 | −0.9 (5) | C25—N4—C26—C22 | −0.3 (5) |
C3—C4—C5—C6 | 179.6 (4) | Ni2—N4—C26—C22 | −175.8 (3) |
C13—C5—C6—C7 | −1.8 (6) | C25—N4—C26—C27 | 179.8 (3) |
C4—C5—C6—C7 | 177.6 (4) | Ni2—N4—C26—C27 | 4.3 (4) |
C5—C6—C7—C8 | −0.6 (6) | C23—C22—C26—N4 | 1.3 (5) |
C6—C7—C8—C9 | −176.8 (4) | C21—C22—C26—N4 | −179.0 (3) |
C6—C7—C8—C12 | 2.7 (6) | C23—C22—C26—C27 | −178.8 (3) |
C12—C8—C9—C10 | −1.2 (6) | C21—C22—C26—C27 | 0.9 (5) |
C7—C8—C9—C10 | 178.3 (4) | C16—N3—C27—C19 | −1.4 (5) |
C8—C9—C10—C11 | 1.6 (6) | Ni2—N3—C27—C19 | −180.0 (3) |
C12—N2—C11—C10 | −1.2 (5) | C16—N3—C27—C26 | 178.4 (3) |
Ni1—N2—C11—C10 | 173.8 (3) | Ni2—N3—C27—C26 | −0.1 (4) |
C12—N2—C11—C14 | 178.4 (3) | C18—C19—C27—N3 | 2.0 (5) |
Ni1—N2—C11—C14 | −6.6 (5) | C20—C19—C27—N3 | −177.4 (3) |
C9—C10—C11—N2 | −0.4 (6) | C18—C19—C27—C26 | −177.9 (3) |
C9—C10—C11—C14 | −179.9 (4) | C20—C19—C27—C26 | 2.7 (5) |
C11—N2—C12—C8 | 1.6 (5) | N4—C26—C27—N3 | −2.9 (4) |
Ni1—N2—C12—C8 | −174.3 (3) | C22—C26—C27—N3 | 177.2 (3) |
C11—N2—C12—C13 | −176.0 (3) | N4—C26—C27—C19 | 177.0 (3) |
Ni1—N2—C12—C13 | 8.1 (4) | C22—C26—C27—C19 | −2.9 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1W1···Cl3i | 0.85 | 2.40 | 3.107 (4) | 140 |
O1—H1W1···Cl4 | 0.85 | 2.80 | 3.106 (3) | 103 |
O2—H1W2···Cl1 | 0.86 | 2.34 | 3.141 (3) | 157 |
O1—H2W1···Cl4 | 0.86 | 2.79 | 3.106 (3) | 104 |
O2—H2W2···Cl2ii | 0.86 | 2.31 | 3.152 (3) | 166 |
C14—H14A···O1 | 0.96 | 2.40 | 3.315 (6) | 159 |
C15—H15A···O2 | 0.96 | 2.28 | 3.223 (6) | 168 |
C17—H17A···Cl4iii | 0.93 | 2.83 | 3.634 (6) | 145 |
Symmetry codes: (i) x+1, y, z; (ii) x−1, y, z; (iii) −x+2, −y+1, −z. |
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