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In the title compound, [Ni(C14H12N4)2](ClO4)2·2CHCl3, each of the two crystallographically independent nickel(II) complex molecules lies on a twofold axis. In each case, the NiII atom is coordinated by the six N atoms of two 2-[3-(2-pyrid­yl)pyrazol-1-ylmeth­yl]pyridine ligands in a distorted octa­hedral geometry. The Ni-Npyrazole bond lengths [1.977 (3)-1.997 (4) Å] are appreciably shorter than the Ni-Npyridine bond lengths [2.133 (4)-2.184 (4) Å].

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805032046/cv6583sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805032046/cv6583Isup2.hkl
Contains datablock I

CCDC reference: 289703

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.008 Å
  • Disorder in solvent or counterion
  • R factor = 0.060
  • wR factor = 0.166
  • Data-to-parameter ratio = 15.2

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT431_ALERT_2_A Short Inter HL..A Contact Cl3 .. Cl3 .. 2.98 Ang.
Author Response: This may be due to the disorder of Cl atoms.

Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98 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 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C7 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 C29 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C30 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 25.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8 PLAT431_ALERT_2_C Short Inter HL..A Contact Cl5' .. O8' .. 3.19 Ang.
Author Response: This may be due to the disorder of Cl atoms.
PLAT431_ALERT_2_C Short Inter HL..A Contact  Cl8    ..  O6'     ..       3.26 Ang.
Author Response: This may be due to the disorder of Cl atoms.
PLAT431_ALERT_2_C Short Inter HL..A Contact  Cl5    ..  O8      ..       3.13 Ang.
Author Response: This may be due to the disorder of Cl atoms.
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         11
            N2  -NI1 -N2  -N3   -143.80  0.40   2.554   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         16
            N2  -NI1 -N2  -C6     61.00  0.40   2.554   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         45
            N6  -NI2 -N6  -C20    57.00  0.30   2.655   1.555   1.555   1.555
PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... #         50
            N6  -NI2 -N6  -N7   -131.70  0.40   2.655   1.555   1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      30.80 Deg.
              O7   -CL2  -O7'     1.555   1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      37.20 Deg.
              O6'  -CL2  -O6      1.555   1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......       9.10 Deg.
              CL5' -C29  -CL5     1.555   1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      41.00 Deg.
              CL3  -C29  -CL3'    1.555   1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      27.90 Deg.
              CL4' -C29  -CL4     1.555   1.555   1.555
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          1
              C28 H24 N8 Ni
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd.  #          6
              C H Cl3

1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 26 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 10 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 13 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.

Bis{2-[3-(2-pyridyl)pyrazol-1-ylmethyl]pyridine}nickel(II) bis(perchlorate) chloroform disolvate top
Crystal data top
[Ni(C14H12N4)2](ClO4)2·2CHCl3F(000) = 3920
Mr = 968.90Dx = 1.571 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 1006 reflections
a = 22.297 (6) Åθ = 3.0–22.6°
b = 17.257 (5) ŵ = 1.05 mm1
c = 23.801 (7) ÅT = 293 K
β = 116.551 (4)°Block, purple
V = 8192 (4) Å30.36 × 0.30 × 0.30 mm
Z = 8
Data collection top
Bruker SMART CCD area-detector
diffractometer
8395 independent reflections
Radiation source: fine-focus sealed tube4749 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.055
φ and ω scansθmax = 26.4°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 2727
Tmin = 0.703, Tmax = 0.743k = 1821
23272 measured reflectionsl = 2927
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.060Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.166H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0746P)2 + 8.6393P]
where P = (Fo2 + 2Fc2)/3
8395 reflections(Δ/σ)max = 0.002
552 parametersΔρmax = 0.62 e Å3
13 restraintsΔρmin = 0.39 e Å3
Special details top

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni10.00001.28352 (5)0.25000.0438 (2)
Ni20.50000.75080 (4)0.25000.0379 (2)
N10.06784 (18)1.2008 (2)0.18690 (17)0.0484 (9)
N20.0297 (2)1.2772 (2)0.1824 (2)0.0614 (11)
N30.0704 (2)1.3185 (3)0.1688 (2)0.0750 (13)
N40.07487 (19)1.3747 (2)0.2917 (2)0.0575 (10)
N50.51876 (16)0.83151 (19)0.19123 (16)0.0433 (8)
N60.41159 (16)0.75905 (19)0.17589 (16)0.0417 (8)
N70.35199 (16)0.7249 (2)0.16049 (16)0.0451 (8)
N80.54203 (18)0.6570 (2)0.21789 (16)0.0443 (8)
Cl10.22217 (5)0.85253 (7)0.21369 (5)0.0527 (3)
Cl20.31475 (7)0.94498 (8)0.07571 (6)0.0636 (4)
Cl30.0704 (9)0.9713 (9)0.0293 (5)0.220 (7)0.446 (12)
Cl40.0794 (6)0.8234 (7)0.0067 (6)0.182 (5)0.446 (12)
Cl50.1768 (6)0.9234 (7)0.0014 (6)0.166 (5)0.446 (12)
Cl3'0.1260 (7)0.9974 (4)0.0607 (4)0.177 (4)0.554 (12)
Cl4'0.0536 (5)0.8596 (10)0.0089 (5)0.267 (8)0.554 (12)
Cl5'0.1765 (5)0.9079 (5)0.0035 (4)0.136 (3)0.554 (12)
Cl60.37780 (18)1.29730 (18)0.09952 (14)0.1876 (13)
Cl70.25214 (15)1.30647 (17)0.08823 (15)0.1887 (14)
Cl80.33786 (12)1.17873 (15)0.04279 (14)0.1537 (10)
C10.1137 (2)1.1599 (3)0.1955 (2)0.0562 (12)
H1A0.11491.16360.23400.067*
C20.1590 (3)1.1127 (3)0.1507 (3)0.0696 (14)
H2A0.19081.08580.15830.083*
C30.1571 (3)1.1056 (3)0.0943 (3)0.0754 (16)
H3A0.18741.07360.06300.090*
C40.1094 (3)1.1467 (3)0.0844 (2)0.0679 (14)
H4A0.10711.14270.04640.081*
C50.0656 (2)1.1936 (3)0.1317 (2)0.0531 (11)
C60.0131 (3)1.2408 (3)0.1274 (2)0.0651 (14)
C70.0034 (3)1.2628 (4)0.0811 (3)0.095 (2)
H7A0.01771.24800.03910.113*
C80.0582 (3)1.3122 (4)0.1093 (3)0.0810 (17)
H8A0.08161.33600.09010.097*
C90.1293 (3)1.3516 (4)0.2194 (3)0.0813 (17)
H9A0.15071.38560.20130.098*
H9B0.16051.30990.24040.098*
C100.1183 (2)1.3977 (3)0.2694 (3)0.0628 (14)
C110.1607 (3)1.4589 (3)0.2958 (3)0.0759 (16)
H11A0.18921.47490.27910.091*
C120.1613 (3)1.4969 (3)0.3469 (4)0.091 (2)
H12A0.19051.53800.36530.110*
C130.1183 (3)1.4729 (3)0.3699 (3)0.0834 (18)
H13A0.11791.49700.40460.100*
C140.0761 (3)1.4128 (3)0.3408 (3)0.0747 (16)
H14A0.04631.39740.35630.090*
C150.5765 (2)0.8667 (3)0.2021 (2)0.0586 (13)
H15A0.61210.86330.24210.070*
C160.5856 (3)0.9075 (3)0.1570 (3)0.0687 (15)
H16A0.62660.93050.16610.082*
C170.5329 (3)0.9137 (3)0.0983 (3)0.0743 (16)
H17A0.53760.94160.06710.089*
C180.4728 (3)0.8782 (3)0.0858 (2)0.0632 (13)
H18A0.43670.88170.04610.076*
C190.4673 (2)0.8375 (2)0.13311 (19)0.0444 (10)
C200.4061 (2)0.7983 (2)0.12562 (19)0.0424 (10)
C210.3416 (2)0.7918 (3)0.0779 (2)0.0581 (13)
H21A0.32430.81450.03830.070*
C220.3086 (2)0.7448 (3)0.1015 (2)0.0567 (12)
H22A0.26400.72950.08040.068*
C230.3396 (2)0.6870 (3)0.2087 (2)0.0524 (11)
H23A0.29800.65810.18830.063*
H23B0.33290.72670.23420.063*
C240.4977 (2)0.6089 (3)0.1751 (2)0.0529 (12)
H24A0.45320.62470.15430.063*
C250.5142 (3)0.5384 (3)0.1603 (3)0.0704 (15)
H25A0.48190.50780.12940.085*
C260.5792 (3)0.5132 (3)0.1915 (3)0.0742 (16)
H26A0.59160.46500.18280.089*
C270.6255 (3)0.5610 (3)0.2359 (2)0.0634 (14)
H27A0.66970.54480.25790.076*
C280.6068 (2)0.6325 (2)0.2482 (2)0.0443 (10)
C290.1283 (3)0.9023 (3)0.0362 (3)0.107 (2)
H29A0.15490.88470.07840.128*
C300.3092 (4)1.2459 (5)0.0986 (4)0.125 (3)
H30A0.28571.22000.13820.150*
O10.25559 (18)0.8520 (2)0.17488 (18)0.0793 (11)
O20.2480 (2)0.7929 (3)0.25923 (19)0.0984 (14)
O30.2340 (2)0.9252 (3)0.2451 (2)0.1095 (16)
O40.15180 (17)0.8421 (2)0.17710 (18)0.0812 (11)
O50.3265 (2)0.8645 (2)0.0641 (2)0.0921 (13)
O6'0.3635 (11)0.9920 (8)0.0317 (8)0.231 (13)0.554 (12)
O7'0.3113 (10)0.9569 (9)0.1350 (5)0.143 (6)0.554 (12)
O8'0.2458 (5)0.9536 (7)0.0905 (11)0.162 (7)0.554 (12)
O60.3821 (5)0.9690 (8)0.0537 (8)0.104 (5)0.446 (12)
O70.2801 (10)0.9736 (12)0.1364 (5)0.145 (9)0.446 (12)
O80.2932 (11)0.9742 (9)0.0326 (8)0.128 (6)0.446 (12)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0397 (4)0.0493 (5)0.0469 (5)0.0000.0234 (4)0.000
Ni20.0344 (4)0.0381 (4)0.0389 (4)0.0000.0142 (3)0.000
N10.049 (2)0.049 (2)0.047 (2)0.0031 (18)0.0219 (18)0.0014 (17)
N20.053 (2)0.073 (3)0.071 (3)0.012 (2)0.039 (2)0.019 (2)
N30.062 (3)0.099 (4)0.076 (3)0.011 (3)0.042 (3)0.027 (3)
N40.049 (2)0.051 (2)0.067 (3)0.0024 (19)0.022 (2)0.000 (2)
N50.038 (2)0.042 (2)0.046 (2)0.0008 (16)0.0162 (17)0.0038 (16)
N60.0354 (19)0.043 (2)0.046 (2)0.0020 (16)0.0181 (16)0.0024 (16)
N70.0345 (19)0.051 (2)0.049 (2)0.0017 (16)0.0177 (17)0.0023 (17)
N80.050 (2)0.043 (2)0.044 (2)0.0021 (17)0.0236 (17)0.0023 (16)
Cl10.0449 (6)0.0615 (7)0.0548 (7)0.0060 (5)0.0252 (5)0.0012 (6)
Cl20.0596 (8)0.0631 (8)0.0684 (9)0.0054 (6)0.0288 (7)0.0121 (7)
Cl30.281 (14)0.251 (11)0.128 (7)0.158 (11)0.092 (9)0.007 (7)
Cl40.262 (14)0.191 (8)0.148 (9)0.040 (8)0.141 (10)0.024 (7)
Cl50.136 (8)0.177 (8)0.190 (10)0.045 (6)0.078 (7)0.064 (7)
Cl3'0.258 (10)0.161 (5)0.131 (6)0.081 (6)0.104 (6)0.021 (4)
Cl4'0.138 (6)0.450 (19)0.149 (7)0.133 (10)0.005 (5)0.116 (10)
Cl5'0.158 (7)0.146 (5)0.117 (5)0.059 (4)0.072 (5)0.009 (4)
Cl60.247 (3)0.173 (3)0.144 (2)0.076 (2)0.089 (2)0.0144 (18)
Cl70.160 (2)0.137 (2)0.191 (3)0.0398 (19)0.009 (2)0.0127 (19)
Cl80.1279 (18)0.1214 (18)0.183 (2)0.0053 (14)0.0441 (17)0.0252 (17)
C10.056 (3)0.063 (3)0.054 (3)0.004 (3)0.028 (2)0.000 (2)
C20.064 (3)0.068 (3)0.077 (4)0.016 (3)0.031 (3)0.006 (3)
C30.071 (4)0.071 (4)0.074 (4)0.015 (3)0.022 (3)0.019 (3)
C40.074 (4)0.078 (4)0.048 (3)0.006 (3)0.023 (3)0.009 (3)
C50.054 (3)0.056 (3)0.049 (3)0.001 (2)0.023 (2)0.003 (2)
C60.061 (3)0.086 (4)0.047 (3)0.002 (3)0.023 (3)0.008 (3)
C70.079 (4)0.148 (6)0.069 (4)0.007 (4)0.043 (3)0.002 (4)
C80.074 (4)0.115 (5)0.073 (4)0.005 (4)0.050 (3)0.022 (4)
C90.067 (4)0.085 (4)0.096 (4)0.016 (3)0.040 (4)0.002 (4)
C100.053 (3)0.054 (3)0.078 (4)0.001 (3)0.027 (3)0.015 (3)
C110.065 (4)0.058 (3)0.103 (5)0.010 (3)0.035 (3)0.014 (3)
C120.075 (4)0.062 (4)0.123 (6)0.018 (3)0.031 (4)0.006 (4)
C130.086 (4)0.062 (4)0.100 (5)0.013 (3)0.039 (4)0.022 (3)
C140.064 (4)0.062 (3)0.101 (5)0.010 (3)0.039 (3)0.011 (3)
C150.048 (3)0.059 (3)0.062 (3)0.010 (2)0.018 (2)0.008 (2)
C160.059 (3)0.066 (3)0.086 (4)0.012 (3)0.037 (3)0.013 (3)
C170.075 (4)0.081 (4)0.073 (4)0.001 (3)0.039 (3)0.029 (3)
C180.060 (3)0.075 (3)0.053 (3)0.002 (3)0.023 (3)0.018 (3)
C190.044 (2)0.044 (2)0.043 (2)0.002 (2)0.017 (2)0.004 (2)
C200.043 (2)0.043 (2)0.036 (2)0.0013 (19)0.013 (2)0.0004 (19)
C210.048 (3)0.077 (3)0.039 (3)0.000 (3)0.010 (2)0.008 (2)
C220.032 (2)0.076 (3)0.048 (3)0.000 (2)0.005 (2)0.003 (2)
C230.041 (2)0.059 (3)0.061 (3)0.005 (2)0.026 (2)0.000 (2)
C240.056 (3)0.052 (3)0.048 (3)0.004 (2)0.021 (2)0.009 (2)
C250.079 (4)0.058 (3)0.065 (3)0.000 (3)0.024 (3)0.020 (3)
C260.088 (4)0.058 (3)0.072 (4)0.022 (3)0.031 (3)0.012 (3)
C270.060 (3)0.058 (3)0.071 (3)0.022 (3)0.028 (3)0.002 (3)
C280.046 (3)0.043 (2)0.048 (3)0.005 (2)0.026 (2)0.005 (2)
C290.127 (6)0.120 (6)0.060 (4)0.021 (5)0.029 (4)0.019 (4)
C300.153 (7)0.109 (6)0.090 (5)0.036 (6)0.035 (5)0.027 (4)
O10.077 (2)0.099 (3)0.083 (3)0.019 (2)0.055 (2)0.017 (2)
O20.101 (3)0.117 (3)0.088 (3)0.043 (3)0.052 (3)0.050 (3)
O30.093 (3)0.097 (3)0.139 (4)0.010 (3)0.052 (3)0.054 (3)
O40.048 (2)0.103 (3)0.083 (3)0.008 (2)0.0209 (19)0.002 (2)
O50.086 (3)0.064 (3)0.126 (3)0.004 (2)0.047 (3)0.023 (2)
O6'0.35 (3)0.078 (9)0.108 (11)0.018 (13)0.038 (14)0.023 (7)
O7'0.186 (16)0.144 (11)0.123 (11)0.036 (10)0.091 (11)0.083 (8)
O8'0.132 (11)0.128 (10)0.27 (2)0.061 (8)0.131 (13)0.055 (11)
O60.065 (7)0.076 (9)0.152 (15)0.040 (6)0.031 (8)0.007 (7)
O70.118 (14)0.158 (14)0.075 (9)0.058 (11)0.033 (9)0.020 (9)
O80.146 (15)0.151 (12)0.131 (13)0.003 (10)0.100 (12)0.029 (10)
Geometric parameters (Å, º) top
Ni1—N21.997 (4)C2—C31.368 (7)
Ni1—N2i1.997 (4)C2—H2A0.9300
Ni1—N1i2.133 (4)C3—C41.382 (8)
Ni1—N12.133 (4)C3—H3A0.9300
Ni1—N4i2.184 (4)C4—C51.377 (7)
Ni1—N42.184 (4)C4—H4A0.9300
Ni2—N61.977 (3)C5—C61.466 (7)
Ni2—N6ii1.977 (3)C6—C71.363 (7)
Ni2—N5ii2.143 (3)C7—C81.391 (8)
Ni2—N52.143 (3)C7—H7A0.9300
Ni2—N8ii2.173 (3)C8—H8A0.9300
Ni2—N82.173 (3)C9—C101.540 (8)
N1—C11.333 (6)C9—H9A0.9700
N1—C51.343 (5)C9—H9B0.9700
N2—N31.304 (5)C10—C111.369 (7)
N2—C61.381 (6)C11—C121.374 (9)
N3—C81.322 (7)C11—H11A0.9300
N3—C91.445 (7)C12—C131.364 (9)
N4—C141.330 (7)C12—H12A0.9300
N4—C101.355 (6)C13—C141.364 (7)
N5—C151.341 (5)C13—H13A0.9300
N5—C191.350 (5)C14—H14A0.9300
N6—C201.331 (5)C15—C161.372 (7)
N6—N71.346 (4)C15—H15A0.9300
N7—C221.345 (5)C16—C171.369 (7)
N7—C231.452 (5)C16—H16A0.9300
N8—C241.343 (5)C17—C181.378 (7)
N8—C281.362 (5)C17—H17A0.9300
Cl1—O21.417 (4)C18—C191.379 (6)
Cl1—O11.423 (3)C18—H18A0.9300
Cl1—O31.423 (4)C19—C201.461 (6)
Cl1—O41.425 (3)C20—C211.382 (6)
Cl2—O6'1.385 (9)C21—C221.373 (7)
Cl2—O71.390 (9)C21—H21A0.9300
Cl2—O7'1.393 (8)C22—H22A0.9300
Cl2—O81.407 (8)C23—C28ii1.505 (6)
Cl2—O61.414 (7)C23—H23A0.9700
Cl2—O51.418 (4)C23—H23B0.9700
Cl2—O8'1.423 (8)C24—C251.363 (7)
Cl3—C291.708 (8)C24—H24A0.9300
Cl4—C291.759 (8)C25—C261.370 (7)
Cl5—C291.722 (8)C25—H25A0.9300
Cl3'—C291.750 (7)C26—C271.374 (7)
Cl4'—C291.695 (8)C26—H26A0.9300
Cl5'—C291.721 (7)C27—C281.375 (6)
Cl6—C301.777 (9)C27—H27A0.9300
Cl7—C301.747 (9)C28—C23ii1.505 (6)
Cl8—C301.660 (8)C29—H29A0.9600
C1—C21.363 (7)C30—H30A0.9599
C1—H1A0.9300
N2—Ni1—N2i173.8 (3)C6—C7—C8106.1 (5)
N2—Ni1—N1i98.32 (15)C6—C7—H7A127.0
N2i—Ni1—N1i77.45 (16)C8—C7—H7A127.0
N2—Ni1—N177.45 (16)N3—C8—C7106.5 (5)
N2i—Ni1—N198.32 (15)N3—C8—H8A126.8
N1i—Ni1—N196.02 (19)C7—C8—H8A126.8
N2—Ni1—N4i97.70 (16)N3—C9—C10116.6 (5)
N2i—Ni1—N4i86.81 (17)N3—C9—H9A108.1
N1i—Ni1—N4i163.72 (15)C10—C9—H9A108.1
N1—Ni1—N4i90.26 (14)N3—C9—H9B108.1
N2—Ni1—N486.81 (17)C10—C9—H9B108.1
N2i—Ni1—N497.70 (16)H9A—C9—H9B107.3
N1i—Ni1—N490.26 (14)N4—C10—C11120.9 (6)
N1—Ni1—N4163.72 (15)N4—C10—C9122.8 (5)
N4i—Ni1—N487.7 (2)C11—C10—C9115.9 (5)
N6—Ni2—N6ii171.7 (2)C10—C11—C12120.4 (6)
N6—Ni2—N5ii97.35 (13)C10—C11—H11A119.8
N6ii—Ni2—N5ii77.21 (13)C12—C11—H11A119.8
N6—Ni2—N577.21 (13)C13—C12—C11118.6 (6)
N6ii—Ni2—N597.35 (13)C13—C12—H12A120.7
N5ii—Ni2—N598.95 (19)C11—C12—H12A120.7
N6—Ni2—N8ii87.29 (14)C12—C13—C14118.5 (6)
N6ii—Ni2—N8ii98.89 (13)C12—C13—H13A120.8
N5ii—Ni2—N8ii90.80 (13)C14—C13—H13A120.8
N5—Ni2—N8ii162.57 (13)N4—C14—C13124.0 (6)
N6—Ni2—N898.89 (13)N4—C14—H14A118.0
N6ii—Ni2—N887.29 (14)C13—C14—H14A118.0
N5ii—Ni2—N8162.57 (13)N5—C15—C16123.1 (5)
N5—Ni2—N890.80 (13)N5—C15—H15A118.4
N8ii—Ni2—N883.70 (19)C16—C15—H15A118.4
C1—N1—C5117.9 (4)C17—C16—C15118.6 (5)
C1—N1—Ni1126.7 (3)C17—C16—H16A120.7
C5—N1—Ni1115.2 (3)C15—C16—H16A120.7
N3—N2—C6106.0 (4)C16—C17—C18119.6 (5)
N3—N2—Ni1133.6 (4)C16—C17—H17A120.2
C6—N2—Ni1116.9 (3)C18—C17—H17A120.2
N2—N3—C8112.9 (5)C17—C18—C19118.9 (5)
N2—N3—C9118.9 (5)C17—C18—H18A120.5
C8—N3—C9126.9 (5)C19—C18—H18A120.5
C14—N4—C10117.6 (5)N5—C19—C18122.0 (4)
C14—N4—Ni1117.8 (3)N5—C19—C20114.2 (4)
C10—N4—Ni1124.5 (4)C18—C19—C20123.8 (4)
C15—N5—C19117.8 (4)N6—C20—C21110.0 (4)
C15—N5—Ni2128.3 (3)N6—C20—C19114.8 (4)
C19—N5—Ni2113.2 (3)C21—C20—C19135.1 (4)
C20—N6—N7107.1 (3)C22—C21—C20105.1 (4)
C20—N6—Ni2119.6 (3)C22—C21—H21A127.4
N7—N6—Ni2132.9 (3)C20—C21—H21A127.4
C22—N7—N6109.5 (4)N7—C22—C21108.2 (4)
C22—N7—C23129.6 (4)N7—C22—H22A125.9
N6—N7—C23119.7 (3)C21—C22—H22A125.9
C24—N8—C28117.2 (4)N7—C23—C28ii116.5 (4)
C24—N8—Ni2116.1 (3)N7—C23—H23A108.2
C28—N8—Ni2124.5 (3)C28ii—C23—H23A108.2
O2—Cl1—O1109.9 (2)N7—C23—H23B108.2
O2—Cl1—O3108.8 (3)C28ii—C23—H23B108.2
O1—Cl1—O3108.6 (3)H23A—C23—H23B107.3
O2—Cl1—O4109.6 (3)N8—C24—C25123.7 (5)
O1—Cl1—O4110.8 (2)N8—C24—H24A118.1
O3—Cl1—O4109.1 (3)C25—C24—H24A118.1
O6'—Cl2—O7117.5 (12)C24—C25—C26119.1 (5)
O6'—Cl2—O7'110.4 (13)C24—C25—H25A120.5
O7—Cl2—O7'30.8 (9)C26—C25—H25A120.5
O6'—Cl2—O869.3 (11)C25—C26—C27118.4 (5)
O7—Cl2—O8114.8 (10)C25—C26—H26A120.8
O7'—Cl2—O8143.5 (9)C27—C26—H26A120.8
O6'—Cl2—O637.2 (11)C26—C27—C28120.5 (5)
O7—Cl2—O6106.6 (12)C26—C27—H27A119.7
O7'—Cl2—O684.3 (10)C28—C27—H27A119.7
O8—Cl2—O6106.1 (9)N8—C28—C27121.0 (4)
O6'—Cl2—O5114.4 (8)N8—C28—C23ii119.9 (4)
O7—Cl2—O5121.3 (9)C27—C28—C23ii118.8 (4)
O7'—Cl2—O5105.2 (7)Cl4'—C29—Cl375.9 (6)
O8—Cl2—O5107.7 (7)Cl4'—C29—Cl5'110.7 (6)
O6—Cl2—O598.2 (6)Cl3—C29—Cl5'122.6 (6)
O6'—Cl2—O8'121.4 (12)Cl4'—C29—Cl5115.5 (7)
O7—Cl2—O8'70.7 (10)Cl3—C29—Cl5115.2 (7)
O7'—Cl2—O8'99.8 (9)Cl5'—C29—Cl59.1 (6)
O8—Cl2—O8'57.3 (8)Cl4'—C29—Cl3'116.9 (7)
O6—Cl2—O8'155.8 (8)Cl3—C29—Cl3'41.0 (5)
O5—Cl2—O8'103.6 (5)Cl5'—C29—Cl3'104.5 (5)
N1—C1—C2123.2 (5)Cl5—C29—Cl3'95.5 (6)
N1—C1—H1A118.4Cl4'—C29—Cl427.9 (7)
C2—C1—H1A118.4Cl3—C29—Cl4103.8 (7)
C1—C2—C3119.0 (5)Cl5'—C29—Cl495.9 (5)
C1—C2—H2A120.5Cl5—C29—Cl4103.5 (6)
C3—C2—H2A120.5Cl3'—C29—Cl4144.8 (6)
C2—C3—C4119.0 (5)Cl4'—C29—H29A119.8
C2—C3—H3A120.5Cl3—C29—H29A114.0
C4—C3—H3A120.5Cl5'—C29—H29A110.4
C5—C4—C3118.7 (5)Cl5—C29—H29A111.9
C5—C4—H4A120.6Cl3'—C29—H29A92.5
C3—C4—H4A120.6Cl4—C29—H29A107.1
N1—C5—C4122.1 (4)Cl8—C30—Cl7110.5 (5)
N1—C5—C6113.4 (4)Cl8—C30—Cl6109.5 (5)
C4—C5—C6124.5 (5)Cl7—C30—Cl6112.9 (5)
C7—C6—N2108.5 (5)Cl8—C30—H30A107.8
C7—C6—C5136.4 (5)Cl7—C30—H30A107.7
N2—C6—C5114.9 (4)Cl6—C30—H30A108.4
N2—Ni1—N1—C1174.6 (4)C2—C3—C4—C50.1 (8)
N2i—Ni1—N1—C10.8 (4)C1—N1—C5—C41.0 (7)
N1i—Ni1—N1—C177.4 (4)Ni1—N1—C5—C4175.4 (4)
N4i—Ni1—N1—C187.6 (4)C1—N1—C5—C6179.7 (4)
N4—Ni1—N1—C1170.5 (5)Ni1—N1—C5—C63.9 (5)
N2—Ni1—N1—C59.4 (3)C3—C4—C5—N10.2 (8)
N2i—Ni1—N1—C5175.2 (3)C3—C4—C5—C6179.5 (5)
N1i—Ni1—N1—C5106.6 (3)N3—N2—C6—C70.8 (6)
N4i—Ni1—N1—C588.4 (3)Ni1—N2—C6—C7160.8 (4)
N4—Ni1—N1—C55.6 (7)N3—N2—C6—C5177.3 (4)
N2i—Ni1—N2—N3143.8 (4)Ni1—N2—C6—C515.7 (6)
N1i—Ni1—N2—N397.0 (4)N1—C5—C6—C7168.1 (7)
N1—Ni1—N2—N3168.6 (5)C4—C5—C6—C711.2 (10)
N4i—Ni1—N2—N380.1 (4)N1—C5—C6—N27.1 (6)
N4—Ni1—N2—N37.2 (4)C4—C5—C6—N2173.6 (5)
N2i—Ni1—N2—C661.0 (4)N2—C6—C7—C81.4 (7)
N1i—Ni1—N2—C6107.8 (4)C5—C6—C7—C8176.8 (6)
N1—Ni1—N2—C613.4 (4)N2—N3—C8—C71.0 (7)
N4i—Ni1—N2—C675.1 (4)C9—N3—C8—C7167.7 (6)
N4—Ni1—N2—C6162.4 (4)C6—C7—C8—N31.4 (7)
C6—N2—N3—C80.2 (6)N2—N3—C9—C1050.7 (7)
Ni1—N2—N3—C8157.3 (4)C8—N3—C9—C10143.4 (6)
C6—N2—N3—C9168.0 (5)C14—N4—C10—C111.3 (7)
Ni1—N2—N3—C934.9 (7)Ni1—N4—C10—C11175.6 (4)
N2—Ni1—N4—C14173.0 (4)C14—N4—C10—C9170.8 (5)
N2i—Ni1—N4—C1411.3 (4)Ni1—N4—C10—C912.3 (7)
N1i—Ni1—N4—C1488.7 (4)N3—C9—C10—N440.3 (8)
N1—Ni1—N4—C14158.3 (5)N3—C9—C10—C11147.2 (5)
N4i—Ni1—N4—C1475.1 (4)N4—C10—C11—C122.0 (8)
N2—Ni1—N4—C103.9 (4)C9—C10—C11—C12170.7 (5)
N2i—Ni1—N4—C10171.8 (4)C10—C11—C12—C130.9 (9)
N1i—Ni1—N4—C1094.4 (4)C11—C12—C13—C140.6 (9)
N1—Ni1—N4—C1018.6 (7)C10—N4—C14—C130.3 (8)
N4i—Ni1—N4—C10101.8 (4)Ni1—N4—C14—C13177.4 (5)
N6—Ni2—N5—C15179.3 (4)C12—C13—C14—N41.3 (9)
N6ii—Ni2—N5—C157.0 (4)C19—N5—C15—C160.6 (7)
N5ii—Ni2—N5—C1585.1 (4)Ni2—N5—C15—C16169.0 (4)
N8ii—Ni2—N5—C15151.6 (4)N5—C15—C16—C171.0 (8)
N8—Ni2—N5—C1580.4 (4)C15—C16—C17—C180.8 (9)
N6—Ni2—N5—C199.3 (3)C16—C17—C18—C190.3 (8)
N6ii—Ni2—N5—C19177.0 (3)C15—N5—C19—C180.0 (6)
N5ii—Ni2—N5—C19104.9 (3)Ni2—N5—C19—C18171.2 (4)
N8ii—Ni2—N5—C1918.4 (6)C15—N5—C19—C20179.3 (4)
N8—Ni2—N5—C1989.6 (3)Ni2—N5—C19—C209.6 (4)
N6ii—Ni2—N6—C2057.0 (3)C17—C18—C19—N50.2 (7)
N5ii—Ni2—N6—C20105.2 (3)C17—C18—C19—C20179.3 (5)
N5—Ni2—N6—C207.6 (3)N7—N6—C20—C212.2 (5)
N8ii—Ni2—N6—C20164.3 (3)Ni2—N6—C20—C21175.5 (3)
N8—Ni2—N6—C2081.1 (3)N7—N6—C20—C19178.2 (3)
N6ii—Ni2—N6—N7131.7 (4)Ni2—N6—C20—C194.8 (5)
N5ii—Ni2—N6—N783.5 (4)N5—C19—C20—N63.7 (5)
N5—Ni2—N6—N7178.9 (4)C18—C19—C20—N6177.0 (4)
N8ii—Ni2—N6—N76.9 (4)N5—C19—C20—C21175.8 (5)
N8—Ni2—N6—N790.1 (4)C18—C19—C20—C213.4 (8)
C20—N6—N7—C222.1 (5)N6—C20—C21—C221.4 (5)
Ni2—N6—N7—C22174.1 (3)C19—C20—C21—C22179.0 (5)
C20—N6—N7—C23171.2 (4)N6—N7—C22—C211.2 (5)
Ni2—N6—N7—C2316.7 (6)C23—N7—C22—C21169.0 (4)
N6—Ni2—N8—C2425.2 (3)C20—C21—C22—N70.1 (5)
N6ii—Ni2—N8—C24160.3 (3)C22—N7—C23—C28ii145.4 (5)
N5ii—Ni2—N8—C24133.3 (4)N6—N7—C23—C28ii48.0 (6)
N5—Ni2—N8—C24102.3 (3)C28—N8—C24—C250.7 (7)
N8ii—Ni2—N8—C2461.1 (3)Ni2—N8—C24—C25164.8 (4)
N6—Ni2—N8—C28172.0 (3)N8—C24—C25—C261.8 (8)
N6ii—Ni2—N8—C282.5 (3)C24—C25—C26—C271.1 (8)
N5ii—Ni2—N8—C2829.5 (6)C25—C26—C27—C280.5 (8)
N5—Ni2—N8—C2894.8 (3)C24—N8—C28—C271.0 (6)
N8ii—Ni2—N8—C28101.8 (3)Ni2—N8—C28—C27161.7 (4)
C5—N1—C1—C21.5 (7)C24—N8—C28—C23ii173.0 (4)
Ni1—N1—C1—C2174.4 (4)Ni2—N8—C28—C23ii24.3 (5)
N1—C1—C2—C31.2 (8)C26—C27—C28—N81.6 (7)
C1—C2—C3—C40.3 (8)C26—C27—C28—C23ii172.5 (5)
Symmetry codes: (i) x, y, z1/2; (ii) x+1, y, z+1/2.
 

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