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Hydrotris(pyrazol­yl)borate (Tp) ligands, also known as scorpionates, are potent tridentate donors that effectively bind metal ions in a face-capping array. Hydro­tris­(3-phenyl­pyrazol­yl)borate enforces a tetra­hedral environment on NiII to model metalloenzymes. The syntheses and structural characterizations of a number of [hydro­tris­(3-phenyl­pyrazol­yl)borato]nickel(II) aryl­oxides were per­formed to provide insight into the environment of the model active site; these com­pounds are chlorido­[hydro­tris­(3-phenyl­pyrazolyl-κN2)borato](3-phenyl-1H-pyrazole-κN2)nickel(II) chloro­form monosolvate, [Ni(C27H22BN6)Cl(C9H8N2)]·CHCl3, (2), [hydro­tris­(3-phenyl­pyrazolyl-κN2)borato](phenolato-κO)nickel(II), [Ni(C27H22BN6)(C6H5O)], (3), (2,6-di­methyl­phenolato-κO)[hydro­tris­(3-phenyl­pyrazolyl-κN2)borato]nickel(II) [Ni(C27H22BN6)(C8H9O)], (4), (4-tert-butyl­phenolato-κO)[hydro­tris­(3-phenyl­pyrazolyl-κN2)borato]nickel(II), [Ni(C27H22BN6)(C10H13O)], (5), and [hydro­tris­(3-phenyl­pyrazolyl-κN2)bor­ato](phenolato-κO)(tetra­hydro­furan-κO)nickel(II) tetra­hydro­furan monosolvate, [Ni(C27H22BN6)(C6H5O)(C4H8O)]·C4H8O, (6). Alkyl groups, e.g. tert-butyl in (5) and methyl in (4), electronically activate the aryl­oxide group to intra­molecular π–π stacking but can be frustrated by steric encumbrance at the inter­acting ring faces. The flexibility at the nickel coordination site, afforded by the uncrowded B atom of the TpPh ligand, allows tetra­hydro­furan coordination in the phenolate compound.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2053229616001789/fo3002sup1.cif
Contains datablocks cpd4, cpd5, cpd6, cpd2, cpd3, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229616001789/fo3002cpd4sup2.hkl
Contains datablock cpd4

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229616001789/fo3002cpd5sup3.hkl
Contains datablock cpd5

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229616001789/fo3002cpd6sup4.hkl
Contains datablock cpd6

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229616001789/fo3002cpd2sup5.hkl
Contains datablock cpd2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2053229616001789/fo3002cpd3sup6.hkl
Contains datablock cpd3

CCDC references: 1450662; 1450661; 1450660; 1450659; 1450658

Computing details top

For all compounds, data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: SHELXTL (Bruker, 2002); software used to prepare material for publication: Mercury (Macrae et al., 2008).

(cpd4) (2,6-Dimethylphenolato-κO)[hydrotris(3-phenylpyrazolyl-κN2)borato]nickel(II) top
Crystal data top
[Ni(C27H22BN6)(C8H9O)]Z = 4
Mr = 621.18F(000) = 1296
Triclinic, P1Dx = 1.339 Mg m3
a = 11.690 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.844 (4) ÅCell parameters from 956 reflections
c = 25.618 (6) Åθ = 2.5–22.9°
α = 91.698 (6)°µ = 0.67 mm1
β = 93.037 (4)°T = 200 K
γ = 119.345 (3)°Block, red
V = 3081.1 (14) Å30.35 × 0.31 × 0.23 mm
Data collection top
Bruker AXS Apex
diffractometer
10889 reflections with I > 2σ(I)
Detector resolution: 836.6 pixels mm-1Rint = 0.037
phi and ω scansθmax = 28.3°, θmin = 0.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1515
Tmin = 0.800, Tmax = 0.862k = 1515
41586 measured reflectionsl = 3434
15266 independent reflections
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)] = 0.045Hydrogen site location: mixed
wR(F2) = 0.115H atoms treated by a mixture of independent and constrained refinement
S = 1.03 w = 1/[σ2(Fo2) + (0.0556P)2 + 0.0842P]
where P = (Fo2 + 2Fc2)/3
15266 reflections(Δ/σ)max = 0.001
803 parametersΔρmax = 0.59 e Å3
0 restraintsΔρmin = 0.22 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.20266 (2)0.28872 (2)0.32572 (2)0.03260 (8)
Ni20.86128 (2)0.60993 (2)0.17419 (2)0.03443 (8)
B10.1845 (2)0.2384 (2)0.20859 (9)0.0384 (5)
H10.181 (2)0.218 (2)0.1661 (8)0.046*
B20.8734 (3)0.5966 (3)0.29189 (10)0.0426 (6)
H20.880 (2)0.594 (2)0.3339 (9)0.051*
O10.20652 (14)0.32746 (14)0.39496 (5)0.0416 (3)
O20.87624 (15)0.63848 (15)0.10522 (5)0.0452 (4)
N10.04499 (15)0.25329 (15)0.27724 (6)0.0331 (4)
N20.06216 (16)0.24227 (16)0.22510 (6)0.0359 (4)
N30.22433 (15)0.14592 (16)0.29091 (6)0.0351 (4)
N40.19584 (15)0.13105 (16)0.23782 (6)0.0366 (4)
N50.33299 (15)0.41053 (16)0.27808 (6)0.0350 (4)
N60.30608 (16)0.36958 (17)0.22620 (6)0.0368 (4)
N70.84815 (16)0.73652 (15)0.22477 (6)0.0358 (4)
N80.86444 (17)0.71676 (16)0.27651 (6)0.0390 (4)
N91.01163 (16)0.61204 (16)0.21720 (7)0.0384 (4)
N100.99749 (17)0.60529 (17)0.26993 (7)0.0410 (4)
N110.73711 (16)0.45452 (16)0.21196 (6)0.0365 (4)
N120.75231 (17)0.47488 (17)0.26530 (7)0.0400 (4)
C10.07449 (19)0.24463 (19)0.27892 (8)0.0349 (4)
C20.1307 (2)0.2301 (2)0.22814 (9)0.0441 (5)
H2A0.21370.22250.21800.053*
C30.0418 (2)0.2291 (2)0.19582 (8)0.0422 (5)
H3A0.05240.22040.15860.051*
C40.0712 (2)0.3229 (2)0.37148 (8)0.0413 (5)
H4A0.01920.38560.37080.050*
C50.1359 (2)0.3146 (2)0.41662 (9)0.0508 (6)
H5A0.08940.37030.44680.061*
C60.2678 (2)0.2250 (3)0.41714 (10)0.0559 (6)
H6A0.31240.21990.44770.067*
C70.3352 (2)0.1434 (2)0.37388 (10)0.0551 (6)
H7A0.42600.08200.37450.066*
C80.2709 (2)0.1504 (2)0.32945 (9)0.0467 (5)
H8A0.31790.09310.29970.056*
C90.13748 (19)0.24073 (19)0.32764 (8)0.0370 (5)
C100.24211 (19)0.04679 (19)0.30469 (8)0.0372 (5)
C110.2209 (2)0.0347 (2)0.26032 (9)0.0451 (5)
H11A0.22510.11280.25880.054*
C120.1927 (2)0.0221 (2)0.21941 (9)0.0441 (5)
H12A0.17400.01030.18380.053*
C130.2652 (3)0.0808 (2)0.37587 (11)0.0623 (7)
H13A0.22300.15630.35260.075*
C140.3060 (3)0.0893 (3)0.42650 (13)0.0811 (9)
H14A0.29130.17090.43750.097*
C150.3666 (3)0.0165 (3)0.46085 (11)0.0672 (8)
H15A0.39310.00890.49570.081*
C160.3890 (2)0.1341 (3)0.44457 (10)0.0565 (6)
H16A0.43180.20910.46810.068*
C170.3492 (2)0.1438 (2)0.39382 (9)0.0468 (5)
H17A0.36640.22630.38290.056*
C180.28538 (19)0.0371 (2)0.35870 (8)0.0396 (5)
C190.44165 (19)0.5283 (2)0.28161 (8)0.0383 (5)
C200.4826 (2)0.5630 (2)0.23154 (9)0.0468 (5)
H20A0.55620.64120.22260.056*
C210.3948 (2)0.4611 (2)0.19791 (9)0.0441 (5)
H21A0.39660.45620.16090.053*
C220.5454 (2)0.7315 (2)0.33961 (11)0.0606 (7)
H22A0.52600.77470.31280.073*
C230.6141 (3)0.7996 (3)0.38590 (14)0.0766 (9)
H23A0.64190.88950.39050.092*
C240.6428 (3)0.7403 (3)0.42499 (12)0.0747 (9)
H24A0.69200.78870.45630.090*
C250.6005 (3)0.6102 (3)0.41901 (11)0.0688 (8)
H25A0.61830.56780.44660.083*
C260.5315 (2)0.5400 (2)0.37277 (9)0.0515 (6)
H26A0.50270.44970.36890.062*
C270.50444 (19)0.6002 (2)0.33229 (9)0.0403 (5)
C280.1812 (2)0.4062 (2)0.47676 (9)0.0462 (5)
C290.1214 (2)0.3801 (3)0.52394 (9)0.0538 (6)
H29A0.14530.44940.54950.065*
C300.0287 (3)0.2565 (3)0.53431 (9)0.0551 (6)
H30A0.01010.24040.56690.066*
C310.0076 (2)0.1560 (2)0.49718 (9)0.0491 (6)
H31A0.07340.07110.50420.059*
C320.0498 (2)0.1760 (2)0.44977 (8)0.0396 (5)
C330.1473 (2)0.3026 (2)0.43997 (7)0.0369 (5)
C340.2781 (3)0.5414 (3)0.46431 (11)0.0676 (8)
H34A0.24580.56350.43230.101*
H34B0.36310.54700.45910.101*
H34C0.28870.60230.49340.101*
C350.0046 (2)0.0676 (2)0.40838 (9)0.0458 (5)
H35A0.06920.01110.42020.069*
H35B0.07730.05130.40200.069*
H35C0.02380.09170.37590.069*
C360.83147 (19)0.84080 (19)0.22426 (8)0.0375 (5)
C370.8392 (2)0.8885 (2)0.27548 (9)0.0465 (5)
H37A0.83160.96180.28630.056*
C380.8597 (2)0.8079 (2)0.30682 (9)0.0463 (5)
H38A0.86920.81540.34400.056*
C390.7013 (2)0.9221 (2)0.17510 (10)0.0506 (6)
H39A0.65320.91100.20510.061*
C400.6720 (2)0.9706 (2)0.13092 (11)0.0569 (7)
H40A0.60490.99380.13090.068*
C410.7397 (3)0.9850 (2)0.08733 (11)0.0591 (7)
H41A0.71861.01740.05700.071*
C420.8385 (3)0.9529 (2)0.08718 (10)0.0534 (6)
H42A0.88480.96280.05680.064*
C430.8700 (2)0.90620 (19)0.13157 (8)0.0426 (5)
H43A0.93900.88560.13160.051*
C440.8014 (2)0.88934 (19)0.17599 (8)0.0390 (5)
C451.1274 (2)0.6172 (2)0.20979 (9)0.0428 (5)
C461.1873 (2)0.6154 (2)0.25811 (10)0.0526 (6)
H46A1.27010.61940.26440.063*
C471.1026 (2)0.6067 (2)0.29433 (10)0.0484 (6)
H47A1.11580.60230.33100.058*
C481.3022 (2)0.6918 (3)0.14700 (11)0.0601 (7)
H48A1.36240.75470.17310.072*
C491.3450 (3)0.6789 (3)0.09911 (13)0.0720 (8)
H49A1.43420.73390.09230.086*
C501.2609 (3)0.5883 (3)0.06176 (12)0.0726 (8)
H50A1.29170.57800.02930.087*
C511.1317 (3)0.5119 (3)0.07097 (12)0.0740 (8)
H51A1.07230.45010.04450.089*
C521.0867 (3)0.5238 (2)0.11837 (11)0.0606 (7)
H52A0.99670.47000.12430.073*
C531.1718 (2)0.6135 (2)0.15723 (10)0.0461 (5)
C540.63004 (19)0.3367 (2)0.20065 (8)0.0382 (5)
C550.5752 (2)0.2840 (2)0.24730 (9)0.0476 (6)
H55A0.49850.20330.25100.057*
C560.6555 (2)0.3733 (2)0.28646 (10)0.0482 (6)
H56A0.64430.36470.32290.058*
C570.4645 (2)0.1802 (3)0.13250 (12)0.0686 (8)
H57A0.39880.15670.15670.082*
C580.4313 (3)0.1196 (3)0.08327 (15)0.0912 (11)
H58A0.34270.05470.07390.109*
C590.5229 (3)0.1505 (3)0.04732 (13)0.0784 (9)
H59A0.49850.10810.01320.094*
C600.6501 (3)0.2434 (3)0.06130 (10)0.0609 (7)
H60A0.71490.26590.03680.073*
C610.6851 (2)0.3049 (2)0.11100 (9)0.0488 (6)
H61A0.77410.36860.12020.059*
C620.5928 (2)0.2752 (2)0.14742 (9)0.0418 (5)
C630.7010 (2)0.6333 (2)0.05087 (8)0.0414 (5)
C640.6613 (3)0.6650 (2)0.00417 (9)0.0528 (6)
H64A0.57150.64160.00280.063*
C650.7496 (3)0.7298 (3)0.03226 (10)0.0624 (7)
H65A0.72020.74850.06450.075*
C660.8797 (3)0.7671 (2)0.02195 (9)0.0607 (7)
H66A0.94020.81290.04710.073*
C670.9260 (2)0.7394 (2)0.02488 (9)0.0485 (6)
C680.8344 (2)0.6692 (2)0.06093 (8)0.0400 (5)
C690.6051 (2)0.5684 (2)0.09144 (9)0.0500 (6)
H69A0.51750.55170.07830.075*
H69B0.63360.62520.12360.075*
H69C0.60150.48620.09890.075*
C701.0695 (3)0.7853 (3)0.03796 (12)0.0709 (8)
H70A1.12100.84030.01070.106*
H70B1.08320.71020.03980.106*
H70D1.09780.83530.07180.106*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.03089 (14)0.03589 (15)0.03206 (14)0.01693 (12)0.00527 (10)0.00329 (10)
Ni20.03557 (15)0.03169 (14)0.03601 (15)0.01620 (12)0.00557 (11)0.00369 (10)
B10.0315 (12)0.0456 (14)0.0345 (12)0.0160 (11)0.0049 (10)0.0012 (10)
B20.0502 (15)0.0432 (14)0.0392 (14)0.0264 (13)0.0051 (11)0.0042 (11)
O10.0405 (8)0.0505 (9)0.0347 (8)0.0228 (7)0.0063 (6)0.0013 (6)
O20.0542 (9)0.0499 (9)0.0367 (8)0.0292 (8)0.0070 (7)0.0049 (7)
N10.0313 (9)0.0343 (9)0.0349 (9)0.0164 (7)0.0069 (7)0.0062 (7)
N20.0321 (9)0.0410 (10)0.0335 (9)0.0170 (8)0.0039 (7)0.0046 (7)
N30.0312 (9)0.0366 (9)0.0368 (9)0.0159 (8)0.0052 (7)0.0028 (7)
N40.0308 (9)0.0401 (10)0.0368 (9)0.0158 (8)0.0060 (7)0.0007 (7)
N50.0285 (8)0.0360 (9)0.0385 (9)0.0142 (7)0.0027 (7)0.0044 (7)
N60.0318 (9)0.0416 (10)0.0349 (9)0.0157 (8)0.0072 (7)0.0066 (7)
N70.0369 (9)0.0326 (9)0.0375 (9)0.0166 (8)0.0046 (7)0.0034 (7)
N80.0464 (10)0.0377 (10)0.0362 (9)0.0231 (8)0.0039 (8)0.0018 (7)
N90.0387 (10)0.0377 (10)0.0426 (10)0.0216 (8)0.0042 (8)0.0037 (7)
N100.0461 (10)0.0391 (10)0.0411 (10)0.0237 (9)0.0002 (8)0.0035 (8)
N110.0376 (9)0.0346 (9)0.0397 (10)0.0193 (8)0.0059 (7)0.0055 (7)
N120.0446 (10)0.0397 (10)0.0414 (10)0.0240 (9)0.0117 (8)0.0092 (8)
C10.0304 (10)0.0301 (10)0.0450 (12)0.0152 (9)0.0055 (9)0.0068 (8)
C20.0364 (12)0.0494 (13)0.0496 (13)0.0240 (11)0.0007 (10)0.0034 (10)
C30.0418 (12)0.0459 (13)0.0376 (12)0.0212 (10)0.0029 (9)0.0033 (9)
C40.0384 (11)0.0426 (12)0.0512 (13)0.0256 (10)0.0086 (10)0.0094 (10)
C50.0543 (15)0.0626 (16)0.0522 (14)0.0409 (13)0.0091 (11)0.0074 (11)
C60.0555 (15)0.0725 (18)0.0592 (16)0.0437 (14)0.0257 (13)0.0212 (13)
C70.0410 (13)0.0569 (15)0.0749 (18)0.0275 (12)0.0220 (12)0.0178 (13)
C80.0373 (12)0.0467 (13)0.0610 (15)0.0238 (11)0.0099 (10)0.0072 (11)
C90.0338 (11)0.0362 (11)0.0506 (13)0.0235 (9)0.0110 (9)0.0130 (9)
C100.0286 (10)0.0307 (10)0.0501 (13)0.0121 (9)0.0100 (9)0.0048 (9)
C110.0427 (12)0.0339 (11)0.0571 (14)0.0174 (10)0.0082 (10)0.0011 (10)
C120.0342 (11)0.0408 (12)0.0500 (13)0.0132 (10)0.0049 (10)0.0093 (10)
C130.0634 (17)0.0415 (14)0.0754 (18)0.0206 (13)0.0019 (14)0.0142 (12)
C140.084 (2)0.0617 (19)0.095 (2)0.0318 (17)0.0050 (18)0.0410 (18)
C150.0574 (17)0.089 (2)0.0599 (17)0.0381 (17)0.0121 (13)0.0296 (16)
C160.0507 (15)0.0782 (19)0.0509 (14)0.0398 (14)0.0032 (11)0.0041 (13)
C170.0466 (13)0.0536 (14)0.0485 (13)0.0310 (12)0.0027 (10)0.0062 (11)
C180.0297 (10)0.0416 (12)0.0500 (13)0.0181 (10)0.0110 (9)0.0122 (10)
C190.0270 (10)0.0350 (11)0.0541 (13)0.0156 (9)0.0074 (9)0.0076 (9)
C200.0359 (12)0.0420 (13)0.0579 (14)0.0142 (10)0.0135 (10)0.0147 (10)
C210.0391 (12)0.0494 (13)0.0443 (12)0.0204 (11)0.0150 (10)0.0151 (10)
C220.0506 (15)0.0450 (14)0.0808 (19)0.0192 (12)0.0087 (13)0.0010 (13)
C230.0590 (18)0.0477 (16)0.100 (2)0.0094 (14)0.0119 (17)0.0221 (16)
C240.0390 (14)0.084 (2)0.0684 (19)0.0062 (15)0.0063 (13)0.0262 (17)
C250.0488 (15)0.087 (2)0.0565 (16)0.0239 (15)0.0019 (12)0.0002 (15)
C260.0381 (12)0.0523 (14)0.0585 (15)0.0185 (11)0.0012 (11)0.0022 (11)
C270.0241 (10)0.0391 (12)0.0541 (13)0.0128 (9)0.0048 (9)0.0003 (10)
C280.0452 (13)0.0510 (14)0.0440 (13)0.0252 (11)0.0042 (10)0.0021 (10)
C290.0597 (15)0.0694 (17)0.0406 (13)0.0391 (14)0.0014 (11)0.0112 (11)
C300.0635 (16)0.0764 (18)0.0385 (13)0.0430 (15)0.0170 (11)0.0112 (12)
C310.0492 (13)0.0577 (15)0.0468 (13)0.0299 (12)0.0121 (11)0.0140 (11)
C320.0395 (11)0.0474 (13)0.0392 (12)0.0269 (10)0.0029 (9)0.0042 (9)
C330.0357 (11)0.0483 (12)0.0317 (10)0.0246 (10)0.0019 (8)0.0014 (9)
C340.0675 (18)0.0539 (16)0.0669 (18)0.0190 (14)0.0114 (14)0.0126 (13)
C350.0442 (13)0.0428 (13)0.0495 (13)0.0206 (11)0.0053 (10)0.0031 (10)
C360.0296 (10)0.0307 (11)0.0502 (13)0.0132 (9)0.0042 (9)0.0030 (9)
C370.0549 (14)0.0391 (12)0.0516 (14)0.0284 (11)0.0040 (11)0.0041 (10)
C380.0558 (14)0.0446 (13)0.0415 (12)0.0272 (12)0.0051 (10)0.0048 (10)
C390.0420 (13)0.0399 (13)0.0687 (16)0.0193 (11)0.0025 (11)0.0059 (11)
C400.0483 (14)0.0469 (14)0.0784 (19)0.0270 (12)0.0107 (13)0.0056 (12)
C410.0726 (18)0.0403 (14)0.0599 (16)0.0263 (13)0.0162 (14)0.0030 (11)
C420.0661 (16)0.0337 (12)0.0543 (15)0.0201 (12)0.0030 (12)0.0021 (10)
C430.0438 (12)0.0294 (11)0.0503 (13)0.0149 (10)0.0013 (10)0.0013 (9)
C440.0351 (11)0.0271 (10)0.0505 (13)0.0126 (9)0.0022 (9)0.0013 (9)
C450.0346 (11)0.0335 (11)0.0620 (14)0.0180 (10)0.0030 (10)0.0048 (10)
C460.0418 (13)0.0451 (13)0.0754 (17)0.0256 (11)0.0039 (12)0.0056 (12)
C470.0520 (14)0.0403 (13)0.0540 (14)0.0245 (11)0.0078 (11)0.0046 (10)
C480.0423 (14)0.0557 (16)0.0809 (19)0.0224 (12)0.0085 (13)0.0087 (13)
C490.0554 (17)0.072 (2)0.096 (2)0.0335 (16)0.0327 (16)0.0228 (17)
C500.079 (2)0.084 (2)0.081 (2)0.0569 (19)0.0295 (17)0.0140 (17)
C510.077 (2)0.077 (2)0.079 (2)0.0466 (18)0.0062 (16)0.0178 (16)
C520.0482 (14)0.0505 (15)0.0838 (19)0.0250 (12)0.0124 (13)0.0109 (13)
C530.0378 (12)0.0403 (12)0.0668 (15)0.0238 (10)0.0089 (11)0.0052 (11)
C540.0313 (10)0.0342 (11)0.0544 (13)0.0194 (9)0.0090 (9)0.0089 (9)
C550.0381 (12)0.0397 (12)0.0678 (16)0.0194 (10)0.0176 (11)0.0162 (11)
C560.0551 (14)0.0464 (13)0.0560 (14)0.0320 (12)0.0253 (12)0.0222 (11)
C570.0386 (14)0.0666 (18)0.090 (2)0.0195 (13)0.0026 (14)0.0084 (15)
C580.0514 (18)0.076 (2)0.124 (3)0.0199 (16)0.0296 (19)0.036 (2)
C590.088 (2)0.076 (2)0.077 (2)0.0503 (19)0.0319 (18)0.0281 (17)
C600.0766 (19)0.0550 (16)0.0564 (16)0.0372 (15)0.0006 (14)0.0013 (12)
C610.0472 (13)0.0392 (12)0.0541 (14)0.0170 (11)0.0024 (11)0.0010 (10)
C620.0347 (11)0.0310 (11)0.0614 (14)0.0178 (9)0.0004 (10)0.0050 (10)
C630.0472 (13)0.0350 (11)0.0393 (12)0.0183 (10)0.0036 (10)0.0007 (9)
C640.0592 (15)0.0475 (14)0.0474 (14)0.0240 (12)0.0056 (11)0.0005 (11)
C650.088 (2)0.0584 (16)0.0407 (14)0.0367 (16)0.0012 (13)0.0068 (11)
C660.083 (2)0.0541 (15)0.0423 (14)0.0290 (15)0.0233 (13)0.0138 (11)
C670.0552 (14)0.0424 (13)0.0462 (13)0.0213 (11)0.0161 (11)0.0056 (10)
C680.0542 (13)0.0351 (11)0.0333 (11)0.0234 (10)0.0081 (9)0.0022 (8)
C690.0474 (13)0.0500 (14)0.0536 (14)0.0241 (12)0.0082 (11)0.0073 (11)
C700.0600 (17)0.0675 (19)0.080 (2)0.0255 (15)0.0254 (15)0.0117 (15)
Geometric parameters (Å, º) top
Ni1—O11.8116 (14)C19—C201.395 (3)
Ni1—N52.0097 (16)C19—C271.473 (3)
Ni1—N32.0186 (17)C20—C211.372 (3)
Ni1—N12.0210 (16)C22—C231.382 (4)
Ni2—O21.8100 (15)C22—C271.389 (3)
Ni2—N92.0135 (17)C23—C241.359 (4)
Ni2—N112.0166 (17)C24—C251.368 (4)
Ni2—N72.0205 (17)C25—C261.389 (3)
B1—N21.534 (3)C26—C271.383 (3)
B1—N61.538 (3)C28—C291.395 (3)
B1—N41.551 (3)C28—C331.402 (3)
B2—N81.539 (3)C28—C341.497 (3)
B2—N101.541 (3)C29—C301.374 (4)
B2—N121.545 (3)C30—C311.377 (3)
O1—C331.342 (2)C31—C321.389 (3)
O2—C681.341 (2)C32—C331.410 (3)
N1—C11.353 (2)C32—C351.499 (3)
N1—N21.373 (2)C36—C371.394 (3)
N2—C31.332 (3)C36—C441.475 (3)
N3—C101.342 (3)C37—C381.365 (3)
N3—N41.368 (2)C39—C401.385 (3)
N4—C121.343 (3)C39—C441.401 (3)
N5—C191.346 (2)C40—C411.369 (4)
N5—N61.367 (2)C41—C421.382 (4)
N6—C211.342 (3)C42—C431.388 (3)
N7—C361.342 (3)C43—C441.389 (3)
N7—N81.372 (2)C45—C461.396 (3)
N8—C381.336 (3)C45—C531.476 (3)
N9—C451.348 (3)C46—C471.363 (3)
N9—N101.369 (2)C48—C491.382 (4)
N10—C471.341 (3)C48—C531.387 (3)
N11—C541.350 (3)C49—C501.356 (4)
N11—N121.367 (2)C50—C511.366 (4)
N12—C561.338 (3)C51—C521.379 (4)
C1—C21.393 (3)C52—C531.381 (3)
C1—C91.473 (3)C54—C551.400 (3)
C2—C31.367 (3)C54—C621.465 (3)
C4—C91.383 (3)C55—C561.368 (3)
C4—C51.395 (3)C57—C581.370 (4)
C5—C61.380 (3)C57—C621.386 (3)
C6—C71.372 (4)C58—C591.367 (4)
C7—C81.379 (3)C59—C601.366 (4)
C8—C91.398 (3)C60—C611.385 (3)
C10—C111.398 (3)C61—C621.383 (3)
C10—C181.475 (3)C63—C641.388 (3)
C11—C121.372 (3)C63—C681.408 (3)
C13—C141.382 (4)C63—C691.501 (3)
C13—C181.386 (3)C64—C651.376 (3)
C14—C151.358 (4)C65—C661.368 (4)
C15—C161.368 (4)C66—C671.403 (3)
C16—C171.384 (3)C67—C681.403 (3)
C17—C181.379 (3)C67—C701.502 (4)
O1—Ni1—N5123.47 (7)C17—C18—C13117.2 (2)
O1—Ni1—N3128.71 (7)C17—C18—C10122.01 (19)
N5—Ni1—N387.41 (7)C13—C18—C10120.8 (2)
O1—Ni1—N1120.17 (6)N5—C19—C20109.24 (19)
N5—Ni1—N193.71 (7)N5—C19—C27122.27 (18)
N3—Ni1—N193.78 (7)C20—C19—C27128.4 (2)
O2—Ni2—N9119.23 (7)C21—C20—C19105.88 (19)
O2—Ni2—N11131.91 (7)N6—C21—C20108.37 (19)
N9—Ni2—N1188.22 (7)C23—C22—C27120.1 (3)
O2—Ni2—N7120.81 (7)C24—C23—C22121.1 (3)
N9—Ni2—N793.60 (7)C23—C24—C25119.6 (3)
N11—Ni2—N793.09 (7)C24—C25—C26120.2 (3)
N2—B1—N6108.06 (18)C27—C26—C25120.6 (3)
N2—B1—N4108.55 (17)C26—C27—C22118.3 (2)
N6—B1—N4108.12 (17)C26—C27—C19120.5 (2)
N8—B2—N10108.14 (18)C22—C27—C19121.0 (2)
N8—B2—N12108.21 (19)C29—C28—C33118.7 (2)
N10—B2—N12107.98 (18)C29—C28—C34121.7 (2)
C33—O1—Ni1149.92 (14)C33—C28—C34119.6 (2)
C68—O2—Ni2149.29 (14)C30—C29—C28121.4 (2)
C1—N1—N2105.83 (15)C29—C30—C31119.5 (2)
C1—N1—Ni1139.98 (14)C30—C31—C32121.5 (2)
N2—N1—Ni1114.00 (11)C31—C32—C33118.6 (2)
C3—N2—N1110.11 (16)C31—C32—C35121.2 (2)
C3—N2—B1129.69 (18)C33—C32—C35120.12 (19)
N1—N2—B1120.09 (16)O1—C33—C28118.65 (19)
C10—N3—N4107.12 (16)O1—C33—C32121.17 (18)
C10—N3—Ni1138.62 (14)C28—C33—C32120.15 (19)
N4—N3—Ni1113.51 (12)N7—C36—C37109.63 (19)
C12—N4—N3109.11 (17)N7—C36—C44123.56 (19)
C12—N4—B1130.71 (18)C37—C36—C44126.71 (19)
N3—N4—B1119.95 (16)C38—C37—C36105.70 (19)
C19—N5—N6106.81 (16)N8—C38—C37108.7 (2)
C19—N5—Ni1138.30 (14)C40—C39—C44120.6 (2)
N6—N5—Ni1114.83 (12)C41—C40—C39120.0 (2)
C21—N6—N5109.68 (17)C40—C41—C42120.5 (2)
C21—N6—B1130.35 (18)C41—C42—C43119.9 (2)
N5—N6—B1119.90 (15)C42—C43—C44120.5 (2)
C36—N7—N8106.27 (16)C43—C44—C39118.5 (2)
C36—N7—Ni2139.69 (14)C43—C44—C36122.69 (19)
N8—N7—Ni2114.00 (12)C39—C44—C36118.8 (2)
C38—N8—N7109.72 (17)N9—C45—C46109.3 (2)
C38—N8—B2129.70 (19)N9—C45—C53122.7 (2)
N7—N8—B2120.37 (16)C46—C45—C53127.8 (2)
C45—N9—N10106.64 (17)C47—C46—C45105.7 (2)
C45—N9—Ni2138.65 (15)N10—C47—C46109.0 (2)
N10—N9—Ni2114.70 (12)C49—C48—C53120.4 (3)
C47—N10—N9109.33 (18)C50—C49—C48120.6 (3)
C47—N10—B2130.61 (19)C49—C50—C51119.7 (3)
N9—N10—B2120.06 (17)C50—C51—C52120.6 (3)
C54—N11—N12106.79 (16)C51—C52—C53120.4 (2)
C54—N11—Ni2138.81 (14)C52—C53—C48118.3 (2)
N12—N11—Ni2113.87 (12)C52—C53—C45120.4 (2)
C56—N12—N11109.47 (18)C48—C53—C45121.0 (2)
C56—N12—B2130.10 (19)N11—C54—C55109.1 (2)
N11—N12—B2120.29 (16)N11—C54—C62122.13 (18)
N1—C1—C2109.56 (18)C55—C54—C62128.4 (2)
N1—C1—C9124.07 (18)C56—C55—C54105.5 (2)
C2—C1—C9126.20 (19)N12—C56—C55109.1 (2)
C3—C2—C1105.78 (19)C58—C57—C62120.8 (3)
N2—C3—C2108.71 (19)C59—C58—C57121.4 (3)
C9—C4—C5120.7 (2)C58—C59—C60118.8 (3)
C6—C5—C4119.6 (2)C59—C60—C61120.4 (3)
C7—C6—C5120.5 (2)C62—C61—C60121.2 (2)
C6—C7—C8120.0 (2)C61—C62—C57117.4 (2)
C7—C8—C9120.8 (2)C61—C62—C54121.45 (19)
C4—C9—C8118.5 (2)C57—C62—C54121.1 (2)
C4—C9—C1123.14 (19)C64—C63—C68119.0 (2)
C8—C9—C1118.4 (2)C64—C63—C69120.7 (2)
N3—C10—C11109.40 (19)C68—C63—C69120.22 (19)
N3—C10—C18122.22 (18)C65—C64—C63121.2 (2)
C11—C10—C18128.3 (2)C66—C65—C64119.8 (2)
C12—C11—C10105.4 (2)C65—C66—C67121.6 (2)
N4—C12—C11108.97 (19)C66—C67—C68118.2 (2)
C14—C13—C18120.6 (3)C66—C67—C70122.2 (2)
C15—C14—C13121.4 (3)C68—C67—C70119.6 (2)
C14—C15—C16119.1 (3)O2—C68—C67119.0 (2)
C15—C16—C17120.0 (3)O2—C68—C63120.76 (19)
C18—C17—C16121.8 (2)C67—C68—C63120.2 (2)
N5—Ni1—O1—C33164.8 (2)C22—C23—C24—C251.5 (4)
N3—Ni1—O1—C3377.8 (3)C23—C24—C25—C261.7 (4)
N1—Ni1—O1—C3346.5 (3)C24—C25—C26—C270.2 (4)
N9—Ni2—O2—C68163.0 (3)C25—C26—C27—C221.4 (3)
N11—Ni2—O2—C6880.0 (3)C25—C26—C27—C19174.6 (2)
N7—Ni2—O2—C6848.3 (3)C23—C22—C27—C261.6 (4)
C1—N1—N2—C30.8 (2)C23—C22—C27—C19174.4 (2)
Ni1—N1—N2—C3175.22 (13)N5—C19—C27—C2649.1 (3)
C1—N1—N2—B1175.72 (18)C20—C19—C27—C26128.0 (2)
Ni1—N1—N2—B18.3 (2)N5—C19—C27—C22135.0 (2)
N6—B1—N2—C3119.9 (2)C20—C19—C27—C2247.9 (3)
N4—B1—N2—C3123.1 (2)C33—C28—C29—C301.5 (4)
N6—B1—N2—N164.4 (2)C34—C28—C29—C30177.4 (2)
N4—B1—N2—N152.6 (2)C28—C29—C30—C310.9 (4)
C10—N3—N4—C121.6 (2)C29—C30—C31—C321.6 (4)
Ni1—N3—N4—C12170.37 (13)C30—C31—C32—C330.0 (3)
C10—N3—N4—B1173.45 (16)C30—C31—C32—C35176.6 (2)
Ni1—N3—N4—B114.6 (2)Ni1—O1—C33—C28149.9 (2)
N2—B1—N4—C12118.2 (2)Ni1—O1—C33—C3228.1 (4)
N6—B1—N4—C12124.8 (2)C29—C28—C33—O1178.91 (19)
N2—B1—N4—N367.9 (2)C34—C28—C33—O12.2 (3)
N6—B1—N4—N349.0 (2)C29—C28—C33—C323.1 (3)
C19—N5—N6—C211.1 (2)C34—C28—C33—C32175.8 (2)
Ni1—N5—N6—C21176.62 (13)C31—C32—C33—O1179.68 (19)
C19—N5—N6—B1178.44 (18)C35—C32—C33—O13.6 (3)
Ni1—N5—N6—B10.7 (2)C31—C32—C33—C282.4 (3)
N2—B1—N6—C21117.2 (2)C35—C32—C33—C28174.3 (2)
N4—B1—N6—C21125.5 (2)N8—N7—C36—C370.9 (2)
N2—B1—N6—N559.5 (2)Ni2—N7—C36—C37176.66 (16)
N4—B1—N6—N557.8 (2)N8—N7—C36—C44175.60 (18)
C36—N7—N8—C380.9 (2)Ni2—N7—C36—C446.8 (3)
Ni2—N7—N8—C38177.40 (14)N7—C36—C37—C380.6 (2)
C36—N7—N8—B2174.31 (18)C44—C36—C37—C38175.8 (2)
Ni2—N7—N8—B27.4 (2)N7—N8—C38—C370.5 (3)
N10—B2—N8—C38122.4 (2)B2—N8—C38—C37174.1 (2)
N12—B2—N8—C38120.9 (2)C36—C37—C38—N80.1 (3)
N10—B2—N8—N763.5 (2)C44—C39—C40—C411.0 (4)
N12—B2—N8—N753.2 (2)C39—C40—C41—C420.7 (4)
C45—N9—N10—C470.2 (2)C40—C41—C42—C430.3 (4)
Ni2—N9—N10—C47179.66 (14)C41—C42—C43—C441.1 (3)
C45—N9—N10—B2179.33 (19)C42—C43—C44—C390.8 (3)
Ni2—N9—N10—B20.2 (2)C42—C43—C44—C36179.61 (19)
N8—B2—N10—C47121.9 (2)C40—C39—C44—C430.2 (3)
N12—B2—N10—C47121.2 (2)C40—C39—C44—C36178.6 (2)
N8—B2—N10—N958.7 (2)N7—C36—C44—C4347.3 (3)
N12—B2—N10—N958.1 (2)C37—C36—C44—C43136.8 (2)
C54—N11—N12—C561.2 (2)N7—C36—C44—C39133.9 (2)
Ni2—N11—N12—C56172.05 (14)C37—C36—C44—C3942.0 (3)
C54—N11—N12—B2174.80 (18)N10—N9—C45—C460.7 (2)
Ni2—N11—N12—B211.9 (2)Ni2—N9—C45—C46179.97 (16)
N8—B2—N12—C56118.9 (2)N10—N9—C45—C53174.42 (18)
N10—B2—N12—C56124.3 (2)Ni2—N9—C45—C534.9 (3)
N8—B2—N12—N1166.1 (2)N9—C45—C46—C471.0 (3)
N10—B2—N12—N1150.8 (2)C53—C45—C46—C47173.8 (2)
N2—N1—C1—C20.8 (2)N9—N10—C47—C460.5 (2)
Ni1—N1—C1—C2173.50 (16)B2—N10—C47—C46179.9 (2)
N2—N1—C1—C9174.65 (18)C45—C46—C47—N100.9 (3)
Ni1—N1—C1—C911.0 (3)C53—C48—C49—C501.0 (4)
N1—C1—C2—C30.6 (2)C48—C49—C50—C512.0 (5)
C9—C1—C2—C3174.8 (2)C49—C50—C51—C521.6 (5)
N1—N2—C3—C20.4 (2)C50—C51—C52—C530.2 (4)
B1—N2—C3—C2175.6 (2)C51—C52—C53—C480.9 (4)
C1—C2—C3—N20.1 (2)C51—C52—C53—C45173.6 (2)
C9—C4—C5—C61.1 (3)C49—C48—C53—C520.5 (4)
C4—C5—C6—C70.7 (4)C49—C48—C53—C45174.0 (2)
C5—C6—C7—C80.1 (4)N9—C45—C53—C5245.9 (3)
C6—C7—C8—C90.5 (3)C46—C45—C53—C52128.3 (3)
C5—C4—C9—C80.8 (3)N9—C45—C53—C48139.7 (2)
C5—C4—C9—C1179.86 (19)C46—C45—C53—C4846.1 (3)
C7—C8—C9—C40.1 (3)N12—N11—C54—C551.6 (2)
C7—C8—C9—C1179.4 (2)Ni2—N11—C54—C55169.00 (16)
N1—C1—C9—C445.0 (3)N12—N11—C54—C62172.36 (17)
C2—C1—C9—C4140.3 (2)Ni2—N11—C54—C6217.0 (3)
N1—C1—C9—C8135.6 (2)N11—C54—C55—C561.4 (2)
C2—C1—C9—C839.1 (3)C62—C54—C55—C56172.1 (2)
N4—N3—C10—C111.8 (2)N11—N12—C56—C550.3 (2)
Ni1—N3—C10—C11167.01 (16)B2—N12—C56—C55175.2 (2)
N4—N3—C10—C18174.80 (17)C54—C55—C56—N120.7 (2)
Ni1—N3—C10—C1816.4 (3)C62—C57—C58—C590.0 (5)
N3—C10—C11—C121.4 (2)C57—C58—C59—C600.3 (5)
C18—C10—C11—C12175.00 (19)C58—C59—C60—C610.0 (4)
N3—N4—C12—C110.8 (2)C59—C60—C61—C620.7 (4)
B1—N4—C12—C11173.58 (19)C60—C61—C62—C571.0 (3)
C10—C11—C12—N40.3 (2)C60—C61—C62—C54177.9 (2)
C18—C13—C14—C150.0 (5)C58—C57—C62—C610.7 (4)
C13—C14—C15—C160.8 (5)C58—C57—C62—C54177.6 (3)
C14—C15—C16—C170.4 (4)N11—C54—C62—C6125.6 (3)
C15—C16—C17—C180.8 (4)C55—C54—C62—C61147.1 (2)
C16—C17—C18—C131.6 (3)N11—C54—C62—C57157.6 (2)
C16—C17—C18—C10179.6 (2)C55—C54—C62—C5729.7 (3)
C14—C13—C18—C171.1 (4)C68—C63—C64—C650.4 (3)
C14—C13—C18—C10180.0 (2)C69—C63—C64—C65177.0 (2)
N3—C10—C18—C1721.0 (3)C63—C64—C65—C661.8 (4)
C11—C10—C18—C17155.0 (2)C64—C65—C66—C670.9 (4)
N3—C10—C18—C13160.2 (2)C65—C66—C67—C681.4 (4)
C11—C10—C18—C1323.8 (3)C65—C66—C67—C70176.9 (2)
N6—N5—C19—C200.9 (2)Ni2—O2—C68—C67147.2 (2)
Ni1—N5—C19—C20175.97 (16)Ni2—O2—C68—C6331.9 (4)
N6—N5—C19—C27176.68 (18)C66—C67—C68—O2178.1 (2)
Ni1—N5—C19—C276.4 (3)C70—C67—C68—O23.6 (3)
N5—C19—C20—C210.4 (2)C66—C67—C68—C632.8 (3)
C27—C19—C20—C21177.0 (2)C70—C67—C68—C63175.6 (2)
N5—N6—C21—C200.9 (2)C64—C63—C68—O2178.94 (19)
B1—N6—C21—C20177.8 (2)C69—C63—C68—O24.4 (3)
C19—C20—C21—N60.3 (3)C64—C63—C68—C672.0 (3)
C27—C22—C23—C240.1 (4)C69—C63—C68—C67174.7 (2)
(cpd5) (4-tert-Butylphenolato-κO)[hydrotris(3-phenylpyrazolyl-κN2)borato]nickel(II) top
Crystal data top
[Ni(C27H22BN6)(C10H13O)]Z = 2
Mr = 649.23F(000) = 680
Triclinic, P1Dx = 1.307 Mg m3
a = 8.428 (3) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.516 (7) ÅCell parameters from 933 reflections
c = 15.064 (7) Åθ = 2.6–20.4°
α = 99.293 (15)°µ = 0.63 mm1
β = 102.679 (16)°T = 200 K
γ = 90.900 (16)°Plate, brown
V = 1649.8 (14) Å30.20 × 0.17 × 0.02 mm
Data collection top
Bruker APEX
diffractometer
4986 reflections with I > 2σ(I)
Detector resolution: 836.6 pixels mm-1Rint = 0.075
ω scansθmax = 28.5°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1111
Tmin = 0.887, Tmax = 0.985k = 1818
22356 measured reflectionsl = 2020
8224 independent reflections
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)] = 0.061Hydrogen site location: mixed
wR(F2) = 0.154H atoms treated by a mixture of independent and constrained refinement
S = 1.01 w = 1/[σ2(Fo2) + (0.0589P)2]
where P = (Fo2 + 2Fc2)/3
8224 reflections(Δ/σ)max = 0.001
434 parametersΔρmax = 0.65 e Å3
66 restraintsΔρmin = 0.46 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni10.40408 (4)0.22502 (3)0.35272 (3)0.03991 (14)
B10.5471 (5)0.2662 (3)0.5582 (3)0.0490 (9)
H10.595 (3)0.283 (2)0.637 (2)0.059*
O10.3492 (2)0.21510 (15)0.22802 (13)0.0452 (5)
N10.3573 (3)0.13757 (18)0.44134 (17)0.0447 (6)
N20.4370 (3)0.16841 (18)0.53106 (17)0.0483 (6)
N30.6435 (3)0.22519 (17)0.40988 (17)0.0425 (6)
N40.6822 (3)0.25432 (18)0.50371 (17)0.0457 (6)
N50.3638 (3)0.34935 (17)0.43814 (16)0.0416 (6)
N60.4399 (3)0.35165 (18)0.52879 (17)0.0446 (6)
C10.2076 (5)0.0027 (3)0.2677 (3)0.0652 (10)
H1A0.29440.04090.26370.078*
C20.1173 (5)0.0609 (3)0.1878 (3)0.0768 (12)
H2A0.13890.05480.12960.092*
C30.0030 (5)0.1273 (3)0.1932 (4)0.0864 (14)
H3A0.06090.17050.13930.104*
C40.0392 (5)0.1308 (3)0.2763 (4)0.0889 (14)
H4A0.12540.17510.27980.107*
C50.0474 (4)0.0710 (3)0.3557 (3)0.0669 (10)
H5A0.01980.07390.41310.080*
C60.1750 (4)0.0063 (2)0.3520 (2)0.0464 (7)
C70.2722 (4)0.0516 (2)0.4387 (2)0.0443 (7)
C80.2963 (4)0.0287 (2)0.5270 (2)0.0546 (9)
H8A0.24970.02720.54500.065*
C90.4007 (4)0.1032 (2)0.5828 (2)0.0543 (9)
H9A0.44100.10790.64740.065*
C100.6884 (4)0.1011 (2)0.2334 (2)0.0514 (8)
H10A0.60920.07170.25880.062*
C110.6942 (5)0.0676 (3)0.1436 (2)0.0600 (9)
H11A0.61760.01710.10620.072*
C120.8137 (5)0.1084 (3)0.1079 (3)0.0679 (11)
H12A0.81910.08540.04570.081*
C130.9242 (5)0.1817 (3)0.1616 (3)0.0683 (10)
H13A1.00690.20840.13700.082*
C140.9149 (4)0.2162 (3)0.2507 (2)0.0544 (9)
H14A0.99070.26740.28760.065*
C150.7955 (4)0.1769 (2)0.2880 (2)0.0447 (7)
C160.7862 (4)0.2146 (2)0.3835 (2)0.0439 (7)
C170.9161 (4)0.2396 (2)0.4610 (2)0.0550 (8)
H17A1.02920.24010.46210.066*
C180.8448 (4)0.2631 (2)0.5343 (2)0.0550 (9)
H18A0.90110.28260.59680.066*
C190.2229 (4)0.4358 (2)0.2661 (2)0.0493 (8)
H19A0.32280.40490.26400.059*
C200.1281 (4)0.4601 (3)0.1863 (3)0.0596 (9)
H20A0.16200.44530.12970.072*
C210.0158 (4)0.5060 (3)0.1892 (3)0.0657 (10)
H21A0.08090.52350.13460.079*
C220.0654 (4)0.5265 (3)0.2711 (3)0.0670 (10)
H22A0.16480.55810.27300.080*
C230.0286 (4)0.5015 (3)0.3500 (3)0.0565 (9)
H23A0.00670.51580.40620.068*
C240.1753 (3)0.4555 (2)0.3490 (2)0.0423 (7)
C250.2751 (4)0.4310 (2)0.4352 (2)0.0423 (7)
C260.2945 (4)0.4853 (2)0.5236 (2)0.0468 (8)
H26A0.24620.54630.54110.056*
C270.3978 (4)0.4329 (2)0.5806 (2)0.0469 (8)
H27A0.43330.45110.64570.056*
C280.5257 (3)0.3105 (2)0.16577 (19)0.0390 (7)
H28A0.57620.34520.22560.047*
C290.5796 (3)0.3314 (2)0.0899 (2)0.0420 (7)
H29A0.66690.38000.09920.050*
C300.5101 (4)0.2837 (2)0.0009 (2)0.0444 (7)
C310.3831 (4)0.2141 (3)0.0080 (2)0.0498 (8)
H31A0.33160.18010.06790.060*
C320.3280 (4)0.1920 (2)0.0671 (2)0.0480 (8)
H32A0.24030.14360.05770.058*
C330.3998 (3)0.2399 (2)0.1559 (2)0.0391 (7)
C340.5719 (4)0.3053 (3)0.0825 (2)0.0592 (9)
C350.7617 (12)0.3116 (12)0.0563 (16)0.076 (3)0.470 (8)
H35A0.80080.24740.04030.115*0.470 (8)
H35B0.80010.36520.00330.115*0.470 (8)
H35C0.80360.32600.10890.115*0.470 (8)
C360.5235 (16)0.4157 (8)0.0970 (8)0.092 (3)0.470 (8)
H36A0.55760.43140.15160.138*0.470 (8)
H36B0.57780.46390.04250.138*0.470 (8)
H36C0.40520.42000.10590.138*0.470 (8)
C370.5115 (18)0.2341 (9)0.1705 (6)0.086 (3)0.470 (8)
H37A0.53110.16520.15990.129*0.470 (8)
H37B0.56920.24950.21690.129*0.470 (8)
H37C0.39440.24070.19270.129*0.470 (8)
C35'0.7455 (11)0.3459 (10)0.0614 (14)0.076 (3)0.530 (8)
H35D0.75320.41560.02940.115*0.530 (8)
H35E0.78210.34350.11910.115*0.530 (8)
H35F0.81470.30520.02190.115*0.530 (8)
C36'0.4495 (13)0.3647 (8)0.1406 (7)0.092 (3)0.530 (8)
H36D0.43720.42960.10380.138*0.530 (8)
H36E0.34400.32690.16030.138*0.530 (8)
H36F0.48870.37560.19510.138*0.530 (8)
C37'0.5712 (16)0.1982 (7)0.1466 (6)0.086 (3)0.530 (8)
H37D0.61240.20700.20090.129*0.530 (8)
H37E0.45980.16830.16630.129*0.530 (8)
H37F0.64110.15390.11160.129*0.530 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0479 (2)0.0362 (2)0.0386 (2)0.00153 (16)0.01667 (18)0.00593 (16)
B10.067 (3)0.041 (2)0.041 (2)0.0007 (18)0.0154 (19)0.0085 (16)
O10.0506 (12)0.0506 (12)0.0378 (12)0.0038 (10)0.0183 (10)0.0067 (9)
N10.0588 (16)0.0369 (13)0.0416 (15)0.0006 (12)0.0184 (13)0.0065 (11)
N20.0714 (18)0.0394 (14)0.0401 (15)0.0002 (13)0.0232 (13)0.0101 (11)
N30.0504 (15)0.0377 (13)0.0405 (15)0.0017 (11)0.0128 (12)0.0063 (11)
N40.0540 (16)0.0424 (14)0.0399 (15)0.0009 (12)0.0090 (12)0.0065 (11)
N50.0526 (15)0.0355 (13)0.0387 (14)0.0014 (11)0.0166 (12)0.0035 (11)
N60.0575 (16)0.0385 (14)0.0386 (15)0.0026 (12)0.0157 (12)0.0033 (11)
C10.077 (3)0.052 (2)0.066 (3)0.0129 (19)0.022 (2)0.0033 (18)
C20.093 (3)0.063 (3)0.066 (3)0.001 (2)0.007 (2)0.002 (2)
C30.063 (3)0.070 (3)0.103 (4)0.000 (2)0.019 (3)0.001 (3)
C40.052 (2)0.082 (3)0.123 (4)0.015 (2)0.001 (3)0.015 (3)
C50.053 (2)0.061 (2)0.092 (3)0.0012 (18)0.018 (2)0.026 (2)
C60.0443 (17)0.0339 (16)0.064 (2)0.0062 (13)0.0164 (16)0.0113 (14)
C70.0490 (18)0.0356 (16)0.057 (2)0.0062 (13)0.0251 (15)0.0147 (14)
C80.071 (2)0.0404 (18)0.065 (2)0.0024 (16)0.0346 (19)0.0197 (16)
C90.077 (2)0.0475 (19)0.048 (2)0.0068 (17)0.0282 (18)0.0163 (16)
C100.058 (2)0.0388 (17)0.063 (2)0.0082 (15)0.0210 (17)0.0136 (15)
C110.071 (2)0.049 (2)0.057 (2)0.0186 (18)0.0130 (19)0.0019 (17)
C120.079 (3)0.078 (3)0.054 (2)0.029 (2)0.030 (2)0.010 (2)
C130.062 (2)0.080 (3)0.076 (3)0.017 (2)0.034 (2)0.025 (2)
C140.0448 (19)0.061 (2)0.065 (2)0.0095 (16)0.0218 (17)0.0186 (18)
C150.0433 (17)0.0391 (16)0.055 (2)0.0116 (14)0.0147 (15)0.0130 (14)
C160.0475 (18)0.0344 (16)0.051 (2)0.0013 (13)0.0114 (15)0.0122 (14)
C170.0460 (19)0.053 (2)0.065 (2)0.0023 (15)0.0089 (17)0.0114 (17)
C180.061 (2)0.0488 (19)0.049 (2)0.0003 (16)0.0009 (17)0.0108 (15)
C190.0480 (18)0.0477 (18)0.056 (2)0.0021 (15)0.0197 (16)0.0080 (15)
C200.066 (2)0.056 (2)0.056 (2)0.0031 (18)0.0159 (19)0.0061 (17)
C210.058 (2)0.069 (2)0.064 (3)0.0026 (19)0.0009 (19)0.013 (2)
C220.044 (2)0.076 (3)0.079 (3)0.0054 (18)0.012 (2)0.010 (2)
C230.048 (2)0.057 (2)0.067 (2)0.0001 (16)0.0214 (18)0.0045 (17)
C240.0403 (16)0.0355 (15)0.0530 (19)0.0051 (13)0.0176 (14)0.0045 (14)
C250.0435 (17)0.0388 (16)0.0483 (19)0.0053 (13)0.0213 (14)0.0041 (14)
C260.0534 (19)0.0366 (16)0.055 (2)0.0011 (14)0.0251 (16)0.0029 (14)
C270.062 (2)0.0423 (17)0.0402 (17)0.0085 (15)0.0253 (15)0.0001 (14)
C280.0439 (17)0.0384 (16)0.0322 (15)0.0043 (13)0.0076 (13)0.0000 (12)
C290.0407 (16)0.0420 (16)0.0445 (18)0.0021 (13)0.0125 (14)0.0071 (13)
C300.0457 (18)0.0551 (19)0.0355 (17)0.0074 (15)0.0124 (14)0.0123 (14)
C310.0506 (19)0.063 (2)0.0320 (17)0.0005 (16)0.0062 (14)0.0002 (15)
C320.0455 (18)0.0529 (19)0.0437 (19)0.0085 (15)0.0114 (15)0.0016 (15)
C330.0428 (16)0.0420 (16)0.0358 (16)0.0078 (13)0.0141 (13)0.0083 (13)
C340.065 (2)0.080 (2)0.0390 (18)0.0069 (18)0.0178 (16)0.0195 (17)
C350.084 (3)0.100 (8)0.059 (3)0.014 (4)0.035 (3)0.030 (6)
C360.125 (8)0.106 (6)0.063 (6)0.033 (5)0.034 (5)0.046 (4)
C370.117 (8)0.111 (6)0.040 (4)0.007 (5)0.037 (4)0.017 (4)
C35'0.084 (3)0.100 (8)0.059 (3)0.014 (4)0.035 (3)0.030 (6)
C36'0.125 (8)0.106 (6)0.063 (6)0.033 (5)0.034 (5)0.046 (4)
C37'0.117 (8)0.111 (6)0.040 (4)0.007 (5)0.037 (4)0.017 (4)
Geometric parameters (Å, º) top
Ni1—O11.815 (2)C12—C131.373 (5)
Ni1—N32.012 (3)C13—C141.368 (5)
Ni1—N12.015 (3)C14—C151.392 (4)
Ni1—N52.026 (2)C15—C161.467 (4)
B1—N41.540 (5)C16—C171.405 (4)
B1—N61.539 (5)C17—C181.366 (5)
B1—N21.547 (5)C19—C241.381 (4)
O1—C331.338 (3)C19—C201.381 (5)
N1—C71.346 (4)C20—C211.377 (5)
N1—N21.365 (3)C21—C221.376 (5)
N2—C91.340 (4)C22—C231.371 (5)
N3—C161.350 (4)C23—C241.394 (4)
N3—N41.369 (3)C24—C251.473 (4)
N4—C181.343 (4)C25—C261.387 (4)
N5—C251.345 (4)C26—C271.373 (4)
N5—N61.370 (3)C28—C331.383 (4)
N6—C271.341 (4)C28—C291.386 (4)
C1—C61.365 (5)C29—C301.387 (4)
C1—C21.386 (5)C30—C311.383 (4)
C2—C31.367 (6)C30—C341.528 (4)
C3—C41.361 (6)C31—C321.385 (4)
C4—C51.379 (6)C32—C331.388 (4)
C5—C61.393 (5)C34—C35'1.503 (9)
C6—C71.473 (4)C34—C371.490 (8)
C7—C81.387 (4)C34—C36'1.526 (7)
C8—C91.367 (5)C34—C361.589 (9)
C10—C151.384 (4)C34—C351.559 (10)
C10—C111.367 (4)C34—C37'1.604 (8)
C11—C121.386 (5)
O1—Ni1—N3116.12 (9)C13—C14—C15120.7 (3)
O1—Ni1—N1133.82 (10)C10—C15—C14118.5 (3)
N3—Ni1—N189.49 (10)C10—C15—C16121.3 (3)
O1—Ni1—N5121.94 (10)C14—C15—C16120.2 (3)
N3—Ni1—N595.14 (10)N3—C16—C17109.6 (3)
N1—Ni1—N590.51 (10)N3—C16—C15122.7 (3)
N4—B1—N6109.3 (3)C17—C16—C15127.6 (3)
N4—B1—N2108.1 (3)C18—C17—C16105.3 (3)
N6—B1—N2107.1 (3)C17—C18—N4109.0 (3)
C33—O1—Ni1143.23 (19)C24—C19—C20121.2 (3)
C7—N1—N2106.7 (2)C21—C20—C19119.6 (3)
C7—N1—Ni1138.5 (2)C22—C21—C20120.1 (4)
N2—N1—Ni1114.73 (18)C21—C22—C23120.0 (3)
C9—N2—N1109.4 (3)C22—C23—C24121.0 (3)
C9—N2—B1130.6 (3)C19—C24—C23118.0 (3)
N1—N2—B1120.0 (2)C19—C24—C25122.2 (3)
C16—N3—N4106.3 (2)C23—C24—C25119.8 (3)
C16—N3—Ni1139.3 (2)N5—C25—C26109.5 (3)
N4—N3—Ni1114.01 (18)N5—C25—C24123.2 (3)
C18—N4—N3109.7 (3)C26—C25—C24127.4 (3)
C18—N4—B1129.8 (3)C27—C26—C25106.0 (3)
N3—N4—B1120.3 (3)N6—C27—C26108.4 (3)
C25—N5—N6106.7 (2)C33—C28—C29121.1 (3)
C25—N5—Ni1139.4 (2)C30—C29—C28122.1 (3)
N6—N5—Ni1113.76 (18)C29—C30—C31116.1 (3)
C27—N6—N5109.5 (2)C29—C30—C34122.0 (3)
C27—N6—B1129.7 (3)C31—C30—C34121.9 (3)
N5—N6—B1120.8 (2)C32—C31—C30122.6 (3)
C6—C1—C2121.7 (4)C31—C32—C33120.6 (3)
C3—C2—C1119.7 (4)O1—C33—C28122.6 (3)
C2—C3—C4119.4 (4)O1—C33—C32119.9 (3)
C3—C4—C5121.0 (4)C28—C33—C32117.5 (3)
C6—C5—C4120.2 (4)C35'—C34—C30115.2 (8)
C1—C6—C5117.9 (3)C37—C34—C30116.3 (6)
C1—C6—C7123.2 (3)C35'—C34—C36'115.0 (7)
C5—C6—C7118.9 (3)C30—C34—C36'110.5 (4)
N1—C7—C8109.4 (3)C37—C34—C36109.5 (5)
N1—C7—C6122.4 (3)C30—C34—C36107.1 (5)
C8—C7—C6128.2 (3)C37—C34—C35110.3 (8)
C9—C8—C7105.8 (3)C30—C34—C35108.3 (9)
N2—C9—C8108.7 (3)C36—C34—C35104.7 (7)
C15—C10—C11121.3 (3)C35'—C34—C37'104.5 (7)
C10—C11—C12119.1 (4)C30—C34—C37'105.6 (5)
C13—C12—C11120.6 (4)C36'—C34—C37'105.0 (5)
C12—C13—C14119.8 (3)
N3—Ni1—O1—C3332.7 (3)Ni1—N3—C16—C17170.2 (2)
N1—Ni1—O1—C33149.8 (3)N4—N3—C16—C15175.5 (2)
N5—Ni1—O1—C3382.4 (3)Ni1—N3—C16—C1512.9 (5)
C7—N1—N2—C90.4 (3)C10—C15—C16—N337.6 (4)
Ni1—N1—N2—C9178.1 (2)C14—C15—C16—N3143.4 (3)
C7—N1—N2—B1180.0 (3)C10—C15—C16—C17138.7 (3)
Ni1—N1—N2—B12.4 (3)C14—C15—C16—C1740.3 (5)
N4—B1—N2—C9120.8 (3)N3—C16—C17—C181.3 (4)
N6—B1—N2—C9121.6 (3)C15—C16—C17—C18175.4 (3)
N4—B1—N2—N159.8 (4)C16—C17—C18—N40.7 (4)
N6—B1—N2—N157.8 (4)N3—N4—C18—C170.2 (4)
C16—N3—N4—C181.0 (3)B1—N4—C18—C17176.0 (3)
Ni1—N3—N4—C18173.0 (2)C24—C19—C20—C210.8 (5)
C16—N3—N4—B1175.6 (3)C19—C20—C21—C220.6 (5)
Ni1—N3—N4—B110.3 (3)C20—C21—C22—C230.1 (6)
N6—B1—N4—C18119.7 (3)C21—C22—C23—C240.2 (5)
N2—B1—N4—C18124.1 (3)C20—C19—C24—C230.5 (4)
N6—B1—N4—N364.4 (3)C20—C19—C24—C25179.4 (3)
N2—B1—N4—N351.8 (4)C22—C23—C24—C190.0 (5)
C25—N5—N6—C270.4 (3)C22—C23—C24—C25179.0 (3)
Ni1—N5—N6—C27175.96 (18)N6—N5—C25—C260.0 (3)
C25—N5—N6—B1177.4 (3)Ni1—N5—C25—C26174.9 (2)
Ni1—N5—N6—B11.0 (3)N6—N5—C25—C24179.8 (2)
N4—B1—N6—C27126.9 (3)Ni1—N5—C25—C245.3 (5)
N2—B1—N6—C27116.3 (3)C19—C24—C25—N535.5 (4)
N4—B1—N6—N556.8 (4)C23—C24—C25—N5145.5 (3)
N2—B1—N6—N560.0 (3)C19—C24—C25—C26144.2 (3)
C6—C1—C2—C33.0 (6)C23—C24—C25—C2634.8 (4)
C1—C2—C3—C44.0 (6)N5—C25—C26—C270.4 (3)
C2—C3—C4—C52.3 (7)C24—C25—C26—C27179.8 (3)
C3—C4—C5—C60.6 (6)N5—N6—C27—C260.7 (3)
C2—C1—C6—C50.2 (5)B1—N6—C27—C26177.4 (3)
C2—C1—C6—C7177.6 (3)C25—C26—C27—N60.7 (3)
C4—C5—C6—C11.6 (5)C33—C28—C29—C300.4 (4)
C4—C5—C6—C7176.0 (3)C28—C29—C30—C310.3 (4)
N2—N1—C7—C80.8 (3)C28—C29—C30—C34178.7 (3)
Ni1—N1—C7—C8177.5 (2)C29—C30—C31—C320.5 (5)
N2—N1—C7—C6177.6 (3)C34—C30—C31—C32178.6 (3)
Ni1—N1—C7—C60.9 (5)C30—C31—C32—C330.0 (5)
C1—C6—C7—N125.6 (5)Ni1—O1—C33—C2814.3 (5)
C5—C6—C7—N1157.0 (3)Ni1—O1—C33—C32163.9 (2)
C1—C6—C7—C8152.5 (3)C29—C28—C33—O1177.3 (3)
C5—C6—C7—C824.9 (5)C29—C28—C33—C320.9 (4)
N1—C7—C8—C90.8 (4)C31—C32—C33—O1177.6 (3)
C6—C7—C8—C9177.5 (3)C31—C32—C33—C280.7 (4)
N1—N2—C9—C80.1 (4)C29—C30—C34—C35'23.8 (7)
B1—N2—C9—C8179.4 (3)C31—C30—C34—C35'155.1 (7)
C7—C8—C9—N20.5 (4)C29—C30—C34—C37167.3 (7)
C15—C10—C11—C122.2 (5)C31—C30—C34—C3711.7 (7)
C10—C11—C12—C130.3 (5)C29—C30—C34—C36'108.4 (6)
C11—C12—C13—C141.1 (6)C31—C30—C34—C36'72.6 (6)
C12—C13—C14—C150.7 (5)C29—C30—C34—C3669.9 (6)
C11—C10—C15—C142.6 (5)C31—C30—C34—C36111.1 (6)
C11—C10—C15—C16178.3 (3)C29—C30—C34—C3542.5 (8)
C13—C14—C15—C101.1 (5)C31—C30—C34—C35136.4 (7)
C13—C14—C15—C16179.8 (3)C29—C30—C34—C37'138.6 (5)
N4—N3—C16—C171.5 (3)C31—C30—C34—C37'40.4 (6)
(cpd6) [Hydrotris(3-phenylpyrazolyl-κN2)borato](phenolato-κO)(tetrahydrofuran-κO)nickel(II) tetrahydrofuran monosolvate top
Crystal data top
[Ni(C27H22BN6)(C6H5O)(C4H8O)]·C4H8ODx = 1.310 Mg m3
Mr = 737.33Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121Cell parameters from 1023 reflections
a = 10.868 (4) Åθ = 2.6–27.8°
b = 11.985 (4) ŵ = 0.57 mm1
c = 28.705 (8) ÅT = 200 K
V = 3739 (2) Å3Block, yellow
Z = 40.29 × 0.18 × 0.14 mm
F(000) = 1552
Data collection top
Bruker APEX
diffractometer
8901 reflections with I > 2σ(I)
Detector resolution: 836.6 pixels mm-1Rint = 0.035
ω scansθmax = 28.2°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1414
Tmin = 0.854, Tmax = 0.927k = 1515
51136 measured reflectionsl = 3838
9233 independent reflections
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.031H-atom parameters constrained
wR(F2) = 0.083 w = 1/[σ2(Fo2) + (0.0509P)2 + 0.3758P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.001
9233 reflectionsΔρmax = 0.37 e Å3
469 parametersΔρmin = 0.17 e Å3
0 restraintsAbsolute structure: Flack x determined using 3794 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons et al., 2013)
Primary atom site location: structure-invariant direct methodsAbsolute structure parameter: 0.02 (1)
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.57355 (2)0.51511 (2)0.10835 (2)0.02717 (7)
B10.6576 (3)0.6948 (2)0.17702 (10)0.0399 (6)
H1A0.68460.75310.19980.048*
N10.50555 (17)0.53410 (18)0.17516 (6)0.0356 (4)
N20.5565 (2)0.62147 (19)0.19878 (7)0.0400 (4)
N30.75639 (17)0.54355 (15)0.12826 (7)0.0307 (4)
N40.76753 (18)0.62099 (18)0.16318 (7)0.0358 (4)
N50.57195 (19)0.68525 (15)0.09548 (6)0.0329 (4)
N60.60729 (19)0.75049 (17)0.13236 (7)0.0374 (4)
O10.59386 (14)0.36318 (13)0.08961 (5)0.0312 (3)
O20.39304 (13)0.51516 (14)0.07999 (5)0.0342 (3)
O30.0871 (3)0.8221 (3)0.21073 (11)0.0950 (11)
C10.4177 (2)0.4903 (2)0.20324 (7)0.0407 (5)
C20.4144 (3)0.5511 (3)0.24507 (9)0.0516 (7)
H2A0.36200.53840.27100.062*
C30.5023 (3)0.6323 (3)0.24083 (9)0.0505 (7)
H3A0.52180.68700.26360.061*
C40.3713 (2)0.3143 (3)0.15845 (10)0.0478 (6)
H4A0.44740.32060.14240.057*
C50.2940 (3)0.2241 (3)0.14918 (13)0.0590 (8)
H5A0.31820.16920.12720.071*
C60.1822 (3)0.2144 (3)0.17198 (14)0.0680 (10)
H6A0.12970.15290.16570.082*
C70.1478 (3)0.2936 (4)0.20355 (13)0.0696 (11)
H7A0.07080.28690.21900.084*
C80.2231 (3)0.3836 (3)0.21348 (11)0.0589 (9)
H8A0.19740.43790.23550.071*
C90.3382 (2)0.3951 (3)0.19093 (9)0.0434 (6)
C100.86937 (19)0.50095 (19)0.12130 (7)0.0311 (4)
C110.9524 (2)0.5494 (2)0.15275 (8)0.0380 (5)
H11A1.03760.53320.15590.046*
C120.8854 (2)0.6247 (2)0.17793 (9)0.0398 (5)
H12A0.91660.67180.20180.048*
C130.8434 (3)0.4366 (2)0.03925 (9)0.0420 (5)
H13A0.78030.49050.03510.050*
C140.8794 (3)0.3695 (3)0.00190 (11)0.0610 (9)
H14A0.84000.37740.02750.073*
C150.9712 (3)0.2925 (3)0.00736 (15)0.0694 (11)
H15A0.99580.24740.01820.083*
C161.0277 (3)0.2806 (3)0.04984 (16)0.0687 (11)
H16A1.09110.22670.05350.082*
C170.9930 (2)0.3464 (2)0.08750 (12)0.0500 (7)
H17A1.03320.33770.11670.060*
C180.8993 (2)0.42504 (19)0.08254 (8)0.0339 (5)
C190.5401 (2)0.7556 (2)0.06087 (9)0.0353 (5)
C200.5526 (3)0.8663 (2)0.07618 (10)0.0439 (6)
H20A0.53500.93240.05910.053*
C210.5958 (2)0.8587 (2)0.12107 (10)0.0444 (6)
H21A0.61440.91990.14090.053*
C220.5596 (3)0.6237 (2)0.00613 (9)0.0442 (5)
H22A0.61740.58120.01120.053*
C230.5308 (3)0.5921 (3)0.05151 (10)0.0540 (7)
H23A0.56870.52830.06490.065*
C240.4469 (3)0.6537 (3)0.07709 (10)0.0554 (8)
H24A0.42840.63320.10830.067*
C250.3905 (3)0.7445 (3)0.05719 (11)0.0531 (7)
H25A0.33130.78560.07440.064*
C260.4194 (3)0.7766 (2)0.01215 (10)0.0445 (5)
H26A0.38050.84010.00100.053*
C270.5050 (2)0.7168 (2)0.01412 (8)0.0356 (5)
C280.7004 (2)0.2875 (2)0.15627 (8)0.0360 (5)
H28A0.67240.34650.17570.043*
C290.7751 (2)0.2047 (2)0.17482 (9)0.0429 (5)
H29A0.79890.20890.20660.052*
C300.8157 (3)0.1159 (2)0.14783 (10)0.0457 (6)
H30A0.86640.05930.16080.055*
C310.7804 (2)0.1119 (2)0.10159 (10)0.0446 (6)
H31A0.80710.05150.08270.054*
C320.7068 (2)0.19423 (19)0.08217 (9)0.0373 (5)
H32A0.68390.18910.05030.045*
C330.66544 (18)0.28520 (17)0.10897 (8)0.0300 (4)
C340.3401 (3)0.4447 (2)0.04424 (9)0.0412 (5)
H34A0.30410.37640.05800.049*
H34B0.40310.42280.02110.049*
C350.2407 (2)0.5163 (2)0.02179 (9)0.0441 (5)
H35A0.27330.55570.00590.053*
H35B0.16960.47000.01220.053*
C360.2035 (3)0.5989 (3)0.05950 (10)0.0521 (7)
H36A0.20620.67620.04740.063*
H36B0.11900.58310.07060.063*
C370.2947 (2)0.5842 (2)0.09832 (9)0.0438 (6)
H37A0.32720.65750.10840.053*
H37B0.25530.54750.12540.053*
C380.1352 (5)0.9197 (4)0.23079 (17)0.0879 (13)
H38A0.12750.91660.26510.105*
H38B0.08960.98580.21940.105*
C390.2652 (5)0.9273 (4)0.21736 (17)0.0938 (15)
H39A0.31900.89570.24190.113*
H39B0.28941.00580.21160.113*
C400.2726 (5)0.8607 (5)0.17405 (19)0.1050 (18)
H40A0.35430.82480.17090.126*
H40B0.25730.90780.14630.126*
C410.1737 (4)0.7757 (4)0.17997 (14)0.0731 (10)
H41A0.13470.75860.14960.088*
H41B0.20800.70580.19300.088*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.02603 (12)0.02875 (12)0.02674 (12)0.00231 (9)0.00001 (10)0.00181 (10)
B10.0404 (14)0.0425 (14)0.0369 (13)0.0047 (11)0.0046 (11)0.0130 (11)
N10.0319 (9)0.0454 (11)0.0294 (8)0.0062 (8)0.0005 (7)0.0016 (8)
N20.0403 (11)0.0495 (11)0.0301 (9)0.0108 (9)0.0003 (8)0.0082 (8)
N30.0298 (8)0.0321 (9)0.0302 (8)0.0005 (7)0.0012 (7)0.0048 (7)
N40.0343 (9)0.0387 (10)0.0344 (9)0.0005 (8)0.0034 (8)0.0069 (8)
N50.0336 (9)0.0299 (8)0.0352 (9)0.0012 (8)0.0031 (8)0.0041 (7)
N60.0404 (10)0.0321 (9)0.0397 (10)0.0016 (8)0.0027 (8)0.0082 (8)
O10.0305 (8)0.0287 (7)0.0346 (7)0.0026 (6)0.0033 (6)0.0028 (6)
O20.0274 (7)0.0368 (8)0.0384 (8)0.0055 (6)0.0037 (6)0.0087 (7)
O30.0722 (17)0.115 (2)0.098 (2)0.0315 (18)0.0311 (16)0.0551 (18)
C10.0334 (10)0.0575 (14)0.0313 (10)0.0138 (12)0.0037 (8)0.0093 (10)
C20.0479 (14)0.0737 (19)0.0332 (11)0.0171 (14)0.0097 (11)0.0030 (11)
C30.0555 (16)0.0664 (18)0.0296 (11)0.0196 (14)0.0020 (11)0.0097 (11)
C40.0353 (12)0.0553 (15)0.0529 (15)0.0001 (11)0.0051 (11)0.0167 (13)
C50.0496 (16)0.0587 (18)0.0686 (19)0.0086 (14)0.0005 (14)0.0185 (15)
C60.0465 (16)0.078 (2)0.079 (2)0.0144 (16)0.0041 (16)0.039 (2)
C70.0337 (14)0.106 (3)0.069 (2)0.0057 (16)0.0048 (13)0.047 (2)
C80.0371 (13)0.092 (2)0.0481 (15)0.0107 (15)0.0086 (11)0.0275 (16)
C90.0317 (11)0.0614 (16)0.0371 (12)0.0058 (11)0.0025 (9)0.0213 (11)
C100.0284 (9)0.0333 (11)0.0317 (9)0.0007 (8)0.0005 (7)0.0050 (8)
C110.0292 (11)0.0469 (13)0.0378 (11)0.0008 (9)0.0053 (9)0.0018 (10)
C120.0358 (11)0.0498 (14)0.0338 (11)0.0052 (10)0.0049 (9)0.0032 (10)
C130.0457 (13)0.0434 (13)0.0371 (12)0.0087 (11)0.0058 (10)0.0027 (10)
C140.071 (2)0.0658 (19)0.0461 (15)0.0294 (17)0.0227 (14)0.0189 (14)
C150.063 (2)0.0581 (18)0.087 (2)0.0285 (16)0.0435 (19)0.0382 (18)
C160.0445 (15)0.0429 (15)0.119 (3)0.0021 (12)0.0287 (19)0.0235 (18)
C170.0357 (12)0.0388 (13)0.0755 (19)0.0023 (11)0.0059 (13)0.0020 (13)
C180.0302 (11)0.0307 (10)0.0410 (12)0.0034 (8)0.0073 (8)0.0005 (9)
C190.0312 (10)0.0307 (10)0.0440 (12)0.0017 (8)0.0000 (9)0.0034 (9)
C200.0463 (14)0.0303 (11)0.0550 (14)0.0013 (10)0.0031 (11)0.0036 (10)
C210.0453 (14)0.0311 (11)0.0568 (15)0.0002 (10)0.0032 (11)0.0088 (10)
C220.0439 (13)0.0477 (13)0.0410 (12)0.0033 (12)0.0060 (11)0.0020 (10)
C230.0628 (17)0.0553 (16)0.0440 (14)0.0034 (14)0.0032 (13)0.0037 (13)
C240.0637 (18)0.0620 (17)0.0406 (13)0.0249 (15)0.0131 (13)0.0137 (12)
C250.0509 (15)0.0528 (16)0.0556 (16)0.0137 (13)0.0193 (13)0.0251 (13)
C260.0414 (12)0.0382 (12)0.0538 (14)0.0028 (11)0.0068 (12)0.0151 (10)
C270.0305 (10)0.0357 (11)0.0404 (11)0.0057 (9)0.0016 (9)0.0085 (9)
C280.0387 (11)0.0346 (11)0.0348 (11)0.0000 (9)0.0041 (9)0.0020 (9)
C290.0452 (13)0.0435 (13)0.0400 (12)0.0013 (11)0.0035 (10)0.0101 (10)
C300.0424 (13)0.0365 (12)0.0581 (16)0.0062 (10)0.0043 (12)0.0119 (11)
C310.0436 (13)0.0312 (11)0.0591 (16)0.0057 (10)0.0008 (11)0.0052 (11)
C320.0367 (11)0.0325 (11)0.0426 (12)0.0017 (9)0.0029 (10)0.0044 (9)
C330.0251 (8)0.0282 (9)0.0367 (10)0.0019 (7)0.0005 (9)0.0024 (9)
C340.0447 (13)0.0338 (11)0.0449 (13)0.0025 (10)0.0071 (11)0.0061 (10)
C350.0423 (12)0.0460 (13)0.0440 (12)0.0082 (11)0.0105 (10)0.0019 (11)
C360.0373 (13)0.0674 (18)0.0516 (15)0.0142 (13)0.0036 (12)0.0043 (14)
C370.0306 (11)0.0554 (15)0.0453 (14)0.0133 (10)0.0002 (9)0.0087 (11)
C380.114 (4)0.059 (2)0.091 (3)0.006 (2)0.020 (3)0.016 (2)
C390.103 (4)0.085 (3)0.093 (3)0.045 (3)0.022 (3)0.010 (2)
C400.076 (3)0.135 (5)0.104 (4)0.037 (3)0.026 (3)0.019 (3)
C410.063 (2)0.087 (3)0.069 (2)0.0084 (19)0.0108 (18)0.025 (2)
Geometric parameters (Å, º) top
Ni1—O11.9115 (16)C10—C111.403 (3)
Ni1—N12.0679 (19)C10—C181.474 (3)
Ni1—N52.072 (2)C11—C121.366 (4)
Ni1—N32.096 (2)C13—C181.390 (4)
Ni1—O22.1239 (16)C13—C141.396 (4)
B1—N41.538 (3)C14—C151.368 (6)
B1—N21.540 (4)C15—C161.373 (6)
B1—N61.546 (4)C16—C171.390 (5)
N1—C11.355 (3)C17—C181.395 (3)
N1—N21.365 (3)C19—C201.404 (3)
N2—C31.350 (3)C19—C271.471 (3)
N3—C101.345 (3)C20—C211.374 (4)
N3—N41.371 (3)C22—C271.391 (4)
N4—C121.350 (3)C22—C231.393 (4)
N5—C191.348 (3)C23—C241.384 (4)
N5—N61.371 (3)C24—C251.374 (5)
N6—C211.342 (3)C25—C261.385 (4)
O1—C331.337 (3)C26—C271.395 (3)
O2—C341.448 (3)C28—C291.388 (3)
O2—C371.451 (3)C28—C331.410 (3)
O3—C381.404 (5)C29—C301.389 (4)
O3—C411.405 (4)C30—C311.382 (4)
C1—C21.405 (4)C31—C321.387 (3)
C1—C91.474 (4)C32—C331.408 (3)
C2—C31.369 (5)C34—C351.523 (4)
C4—C91.392 (4)C35—C361.522 (4)
C4—C51.394 (4)C36—C371.502 (4)
C5—C61.386 (5)C38—C391.468 (7)
C6—C71.364 (6)C39—C401.479 (7)
C7—C81.384 (6)C40—C411.492 (6)
C8—C91.415 (4)
O1—Ni1—N1114.03 (8)C4—C9—C8117.9 (3)
O1—Ni1—N5152.63 (7)C4—C9—C1123.2 (2)
N1—Ni1—N593.10 (8)C8—C9—C1118.9 (3)
O1—Ni1—N397.02 (7)N3—C10—C11109.6 (2)
N1—Ni1—N393.91 (8)N3—C10—C18123.25 (19)
N5—Ni1—N384.06 (8)C11—C10—C18126.8 (2)
O1—Ni1—O289.95 (6)C12—C11—C10105.7 (2)
N1—Ni1—O291.45 (7)N4—C12—C11108.5 (2)
N5—Ni1—O285.62 (7)C18—C13—C14120.4 (3)
N3—Ni1—O2168.61 (7)C15—C14—C13120.3 (3)
N4—B1—N2109.3 (2)C14—C15—C16119.9 (3)
N4—B1—N6108.0 (2)C15—C16—C17120.7 (3)
N2—B1—N6109.3 (2)C16—C17—C18120.1 (3)
C1—N1—N2106.71 (19)C13—C18—C17118.5 (2)
C1—N1—Ni1139.53 (18)C13—C18—C10121.1 (2)
N2—N1—Ni1113.58 (15)C17—C18—C10120.1 (2)
C3—N2—N1109.9 (2)N5—C19—C20109.6 (2)
C3—N2—B1128.3 (2)N5—C19—C27122.7 (2)
N1—N2—B1121.74 (18)C20—C19—C27127.6 (2)
C10—N3—N4106.55 (17)C21—C20—C19105.3 (2)
C10—N3—Ni1139.79 (15)N6—C21—C20108.8 (2)
N4—N3—Ni1113.14 (14)C27—C22—C23120.9 (3)
C12—N4—N3109.6 (2)C24—C23—C22120.0 (3)
C12—N4—B1129.5 (2)C25—C24—C23119.7 (3)
N3—N4—B1120.62 (19)C24—C25—C26120.5 (3)
C19—N5—N6106.50 (19)C25—C26—C27120.9 (3)
C19—N5—Ni1138.51 (16)C22—C27—C26118.1 (2)
N6—N5—Ni1114.90 (14)C22—C27—C19121.6 (2)
C21—N6—N5109.8 (2)C26—C27—C19120.2 (2)
C21—N6—B1130.6 (2)C29—C28—C33120.9 (2)
N5—N6—B1119.56 (19)C28—C29—C30121.3 (2)
C33—O1—Ni1128.03 (14)C31—C30—C29118.3 (2)
C34—O2—C37107.27 (18)C30—C31—C32121.5 (2)
C34—O2—Ni1129.67 (14)C31—C32—C33121.0 (2)
C37—O2—Ni1122.81 (14)O1—C33—C32120.0 (2)
C38—O3—C41109.8 (3)O1—C33—C28122.9 (2)
N1—C1—C2109.0 (2)C32—C33—C28117.1 (2)
N1—C1—C9124.8 (2)O2—C34—C35104.7 (2)
C2—C1—C9126.3 (2)C36—C35—C34104.7 (2)
C3—C2—C1106.0 (2)C37—C36—C35106.0 (2)
N2—C3—C2108.4 (3)O2—C37—C36106.5 (2)
C9—C4—C5120.8 (3)O3—C38—C39107.6 (4)
C6—C5—C4120.2 (4)C38—C39—C40103.9 (4)
C7—C6—C5119.7 (4)C39—C40—C41103.5 (4)
C6—C7—C8121.2 (3)O3—C41—C40106.5 (4)
C7—C8—C9120.3 (4)
C1—N1—N2—C30.2 (3)C13—C14—C15—C160.4 (4)
Ni1—N1—N2—C3176.36 (17)C14—C15—C16—C170.3 (5)
C1—N1—N2—B1177.9 (2)C15—C16—C17—C180.5 (4)
Ni1—N1—N2—B11.7 (3)C14—C13—C18—C170.9 (4)
N4—B1—N2—C3124.6 (3)C14—C13—C18—C10175.1 (2)
N6—B1—N2—C3117.4 (3)C16—C17—C18—C130.8 (4)
N4—B1—N2—N157.7 (3)C16—C17—C18—C10175.1 (2)
N6—B1—N2—N160.3 (3)N3—C10—C18—C1334.8 (3)
C10—N3—N4—C120.9 (3)C11—C10—C18—C13137.6 (2)
Ni1—N3—N4—C12172.56 (16)N3—C10—C18—C17151.0 (2)
C10—N3—N4—B1174.0 (2)C11—C10—C18—C1736.6 (3)
Ni1—N3—N4—B112.5 (3)N6—N5—C19—C201.3 (3)
N2—B1—N4—C12119.5 (3)Ni1—N5—C19—C20174.9 (2)
N6—B1—N4—C12121.7 (3)N6—N5—C19—C27175.6 (2)
N2—B1—N4—N366.7 (3)Ni1—N5—C19—C278.2 (4)
N6—B1—N4—N352.1 (3)N5—C19—C20—C211.2 (3)
C19—N5—N6—C210.9 (3)C27—C19—C20—C21175.5 (2)
Ni1—N5—N6—C21176.32 (17)N5—N6—C21—C200.2 (3)
C19—N5—N6—B1176.1 (2)B1—N6—C21—C20176.5 (2)
Ni1—N5—N6—B16.6 (3)C19—C20—C21—N60.6 (3)
N4—B1—N6—C21120.3 (3)C27—C22—C23—C240.1 (5)
N2—B1—N6—C21120.9 (3)C22—C23—C24—C251.3 (5)
N4—B1—N6—N556.0 (3)C23—C24—C25—C261.7 (4)
N2—B1—N6—N562.8 (3)C24—C25—C26—C270.8 (4)
N2—N1—C1—C20.3 (3)C23—C22—C27—C260.8 (4)
Ni1—N1—C1—C2174.9 (2)C23—C22—C27—C19176.0 (3)
N2—N1—C1—C9178.9 (2)C25—C26—C27—C220.4 (4)
Ni1—N1—C1—C94.4 (4)C25—C26—C27—C19176.4 (2)
N1—C1—C2—C30.3 (3)N5—C19—C27—C2235.0 (3)
C9—C1—C2—C3178.9 (2)C20—C19—C27—C22141.4 (3)
N1—N2—C3—C20.0 (3)N5—C19—C27—C26148.3 (2)
B1—N2—C3—C2177.9 (2)C20—C19—C27—C2635.4 (4)
C1—C2—C3—N20.2 (3)C33—C28—C29—C301.4 (4)
C9—C4—C5—C60.6 (5)C28—C29—C30—C310.4 (4)
C4—C5—C6—C70.1 (5)C29—C30—C31—C320.3 (4)
C5—C6—C7—C80.4 (5)C30—C31—C32—C330.1 (4)
C6—C7—C8—C90.1 (5)Ni1—O1—C33—C32155.42 (16)
C5—C4—C9—C81.0 (4)Ni1—O1—C33—C2826.2 (3)
C5—C4—C9—C1178.1 (3)C31—C32—C33—O1179.5 (2)
C7—C8—C9—C40.8 (4)C31—C32—C33—C281.1 (3)
C7—C8—C9—C1178.4 (2)C29—C28—C33—O1179.9 (2)
N1—C1—C9—C425.0 (4)C29—C28—C33—C321.7 (3)
C2—C1—C9—C4155.9 (3)C37—O2—C34—C3534.0 (3)
N1—C1—C9—C8156.0 (2)Ni1—O2—C34—C35151.76 (17)
C2—C1—C9—C823.2 (4)O2—C34—C35—C3625.8 (3)
N4—N3—C10—C111.5 (2)C34—C35—C36—C378.8 (3)
Ni1—N3—C10—C11169.12 (19)C34—O2—C37—C3628.6 (3)
N4—N3—C10—C18172.0 (2)Ni1—O2—C37—C36156.69 (19)
Ni1—N3—C10—C1817.3 (4)C35—C36—C37—O211.3 (3)
N3—C10—C11—C121.6 (3)C41—O3—C38—C398.4 (6)
C18—C10—C11—C12171.7 (2)O3—C38—C39—C4023.9 (6)
N3—N4—C12—C110.1 (3)C38—C39—C40—C4129.4 (6)
B1—N4—C12—C11174.4 (2)C38—O3—C41—C4010.7 (6)
C10—C11—C12—N41.0 (3)C39—C40—C41—O325.1 (6)
C18—C13—C14—C150.7 (4)
(cpd2) Chlorido[hydrotris(3-phenylpyrazolyl-κN2)borato](3-phenyl-1H-pyrazole-κN2)nickel(II) chloroform monosolvate top
Crystal data top
[Ni(C27H23BN6)Cl(C9H8N2)]·CHCl3Z = 2
Mr = 799.02F(000) = 820
Triclinic, P1Dx = 1.454 Mg m3
a = 11.941 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 11.986 (2) ÅCell parameters from 993 reflections
c = 14.034 (2) Åθ = 1.9–25.2°
α = 80.223 (2)°µ = 0.87 mm1
β = 81.483 (2)°T = 200 K
γ = 67.810 (2)°Block, green
V = 1825.0 (5) Å30.59 × 0.46 × 0.20 mm
Data collection top
Bruker APEX
diffractometer
7153 reflections with I > 2σ(I)
Detector resolution: 836.6 pixels mm-1Rint = 0.033
ω scansθmax = 28.3°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1515
Tmin = 0.629, Tmax = 0.849k = 1515
24843 measured reflectionsl = 1818
9015 independent reflections
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)] = 0.055Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.163H-atom parameters constrained
S = 1.00 w = 1/[σ2(Fo2) + (0.0921P)2 + 1.5915P]
where P = (Fo2 + 2Fc2)/3
9015 reflections(Δ/σ)max < 0.001
479 parametersΔρmax = 0.83 e Å3
126 restraintsΔρmin = 0.97 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Ni0.93221 (3)0.72164 (3)0.22103 (2)0.02570 (11)
B11.1835 (3)0.5644 (3)0.1324 (2)0.0295 (6)
H11.26490.51380.10330.035*
N11.02432 (19)0.53455 (19)0.26603 (16)0.0284 (4)
N21.13969 (19)0.4905 (2)0.22087 (16)0.0291 (4)
N30.96987 (19)0.66797 (19)0.08485 (16)0.0278 (4)
N41.0893 (2)0.6074 (2)0.05714 (16)0.0299 (5)
N51.0903 (2)0.7542 (2)0.21472 (16)0.0283 (4)
N61.19030 (19)0.6773 (2)0.16738 (16)0.0289 (4)
N70.7674 (2)0.9871 (2)0.20573 (17)0.0303 (5)
H70.73380.97420.26470.036*
N80.8498 (2)0.8985 (2)0.15729 (16)0.0295 (5)
C11.0148 (2)0.4463 (2)0.33621 (19)0.0298 (5)
C21.1251 (3)0.3471 (3)0.3378 (2)0.0393 (6)
H2A1.14370.27360.38090.047*
C31.2003 (3)0.3791 (3)0.2640 (2)0.0359 (6)
H3A1.28200.33020.24620.043*
C40.7924 (3)0.4902 (3)0.3536 (2)0.0365 (6)
H4A0.79190.51320.28540.044*
C50.6849 (3)0.4941 (3)0.4095 (2)0.0445 (7)
H5A0.61120.52070.37980.053*
C60.6860 (3)0.4589 (3)0.5090 (3)0.0478 (8)
H6A0.61270.46230.54770.057*
C70.7936 (3)0.4190 (3)0.5514 (2)0.0466 (8)
H7A0.79420.39370.61930.056*
C80.9005 (3)0.4153 (3)0.4962 (2)0.0365 (6)
H8A0.97410.38700.52620.044*
C90.9006 (3)0.4530 (2)0.39643 (19)0.0301 (5)
C100.9080 (2)0.6862 (2)0.00717 (19)0.0286 (5)
C110.9892 (3)0.6395 (3)0.0719 (2)0.0327 (6)
H11A0.97060.64140.13580.039*
C121.1016 (3)0.5906 (3)0.0370 (2)0.0330 (6)
H12A1.17600.55130.07330.040*
C130.7052 (3)0.7240 (3)0.1000 (2)0.0419 (7)
H13A0.74450.68300.15690.050*
C140.5785 (3)0.7687 (4)0.1044 (3)0.0531 (9)
H14A0.53220.75890.16420.064*
C150.5211 (3)0.8265 (4)0.0227 (3)0.0601 (10)
H15A0.43490.85630.02570.072*
C160.5870 (4)0.8413 (4)0.0624 (3)0.0646 (11)
H16A0.54640.88170.11880.078*
C170.7145 (3)0.7977 (3)0.0684 (3)0.0491 (8)
H17A0.75970.80840.12870.059*
C180.7741 (2)0.7390 (2)0.0137 (2)0.0322 (6)
C191.1206 (2)0.8466 (2)0.23042 (19)0.0309 (5)
C201.2402 (3)0.8274 (3)0.1935 (2)0.0378 (6)
H20A1.28450.87840.19470.045*
C211.2809 (2)0.7200 (3)0.1550 (2)0.0338 (6)
H21A1.36000.68210.12460.041*
C220.9775 (3)0.9292 (3)0.3717 (2)0.0410 (7)
H22A0.98830.84870.40060.049*
C230.9022 (3)1.0272 (3)0.4196 (3)0.0492 (8)
H23A0.86271.01320.48180.059*
C240.8843 (3)1.1445 (3)0.3778 (3)0.0482 (8)
H24A0.83201.21100.41070.058*
C250.9425 (3)1.1647 (3)0.2881 (3)0.0509 (8)
H25A0.93011.24550.25880.061*
C261.0192 (3)1.0677 (3)0.2403 (2)0.0439 (7)
H26A1.06011.08230.17880.053*
C271.0367 (3)0.9494 (2)0.2818 (2)0.0323 (6)
C280.7422 (2)1.0979 (2)0.1536 (2)0.0314 (5)
C290.8125 (3)1.0790 (3)0.0661 (2)0.0378 (6)
H29A0.81591.13860.01280.045*
C300.8771 (3)0.9547 (3)0.0725 (2)0.0344 (6)
H30A0.93340.91510.02250.041*
C310.5925 (3)1.2119 (3)0.2808 (2)0.0447 (7)
H31A0.60461.13790.32250.054*
C320.5116 (3)1.3195 (3)0.3121 (3)0.0510 (8)
H32A0.46791.31910.37440.061*
C330.4949 (3)1.4275 (3)0.2521 (3)0.0485 (8)
H33A0.43931.50160.27320.058*
C340.5589 (3)1.4283 (3)0.1613 (3)0.0550 (9)
H34A0.54821.50280.12060.066*
C350.6386 (3)1.3196 (3)0.1303 (3)0.0450 (7)
H35A0.68151.32010.06770.054*
C360.6565 (2)1.2100 (2)0.1895 (2)0.0329 (6)
Cl10.79898 (7)0.76430 (6)0.35863 (5)0.04151 (18)
C370.5518 (6)0.0874 (5)0.5983 (4)0.0772 (15)0.871 (2)
H37A0.46810.12260.57620.093*0.871 (2)
Cl20.61870 (19)0.19923 (17)0.57551 (14)0.0847 (5)0.871 (2)
Cl30.64452 (15)0.03559 (16)0.53113 (14)0.0959 (5)0.871 (2)
Cl40.5449 (2)0.0315 (2)0.72033 (12)0.1252 (8)0.871 (2)
C37'0.543 (3)0.0879 (17)0.6232 (18)0.134 (15)0.129 (2)
H37B0.46920.10040.67060.160*0.129 (2)
Cl2'0.5837 (16)0.2190 (12)0.5986 (11)0.0847 (5)0.129 (2)
Cl3'0.5215 (10)0.0482 (10)0.5117 (9)0.0959 (5)0.129 (2)
Cl4'0.6723 (14)0.0336 (12)0.6687 (8)0.1252 (8)0.129 (2)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.02570 (18)0.02418 (18)0.02721 (18)0.00854 (13)0.00090 (12)0.00562 (12)
B10.0242 (13)0.0291 (14)0.0342 (15)0.0079 (11)0.0001 (11)0.0078 (12)
N10.0278 (11)0.0252 (10)0.0320 (11)0.0089 (9)0.0020 (9)0.0057 (8)
N20.0260 (10)0.0274 (11)0.0327 (11)0.0073 (9)0.0030 (8)0.0062 (9)
N30.0265 (10)0.0270 (10)0.0299 (11)0.0083 (9)0.0019 (8)0.0075 (8)
N40.0277 (11)0.0301 (11)0.0322 (11)0.0095 (9)0.0007 (9)0.0099 (9)
N50.0279 (11)0.0280 (11)0.0303 (11)0.0103 (9)0.0027 (8)0.0069 (9)
N60.0258 (10)0.0289 (11)0.0323 (11)0.0097 (9)0.0035 (8)0.0047 (9)
N70.0294 (11)0.0275 (11)0.0320 (11)0.0084 (9)0.0006 (9)0.0059 (9)
N80.0275 (11)0.0269 (11)0.0331 (11)0.0074 (9)0.0016 (9)0.0077 (9)
C10.0335 (13)0.0267 (12)0.0315 (13)0.0113 (10)0.0085 (10)0.0042 (10)
C20.0391 (15)0.0303 (14)0.0467 (17)0.0117 (12)0.0102 (13)0.0034 (12)
C30.0295 (13)0.0287 (13)0.0467 (16)0.0052 (11)0.0078 (12)0.0058 (12)
C40.0401 (15)0.0364 (15)0.0347 (14)0.0162 (12)0.0078 (12)0.0004 (11)
C50.0367 (16)0.0479 (18)0.0510 (18)0.0170 (14)0.0038 (13)0.0076 (14)
C60.0469 (18)0.0517 (19)0.0476 (18)0.0232 (15)0.0103 (14)0.0139 (15)
C70.061 (2)0.0495 (18)0.0326 (15)0.0259 (16)0.0028 (14)0.0066 (13)
C80.0450 (16)0.0335 (14)0.0343 (14)0.0173 (12)0.0077 (12)0.0021 (11)
C90.0375 (14)0.0237 (12)0.0322 (13)0.0137 (10)0.0049 (11)0.0043 (10)
C100.0329 (13)0.0275 (12)0.0291 (12)0.0141 (10)0.0050 (10)0.0040 (10)
C110.0399 (15)0.0364 (14)0.0267 (13)0.0179 (12)0.0030 (11)0.0074 (10)
C120.0357 (14)0.0352 (14)0.0306 (13)0.0158 (12)0.0047 (11)0.0107 (11)
C130.0339 (15)0.0497 (18)0.0420 (16)0.0163 (13)0.0052 (12)0.0015 (13)
C140.0347 (16)0.062 (2)0.064 (2)0.0195 (16)0.0013 (15)0.0126 (18)
C150.0337 (17)0.064 (2)0.081 (3)0.0141 (16)0.0125 (17)0.007 (2)
C160.050 (2)0.074 (3)0.067 (3)0.0166 (19)0.0307 (19)0.006 (2)
C170.0460 (18)0.057 (2)0.0421 (17)0.0145 (16)0.0147 (14)0.0015 (15)
C180.0332 (14)0.0301 (13)0.0375 (14)0.0131 (11)0.0084 (11)0.0067 (11)
C190.0340 (14)0.0314 (13)0.0309 (13)0.0143 (11)0.0088 (10)0.0029 (10)
C200.0354 (15)0.0402 (15)0.0448 (16)0.0199 (12)0.0078 (12)0.0058 (12)
C210.0271 (13)0.0372 (14)0.0384 (15)0.0129 (11)0.0044 (11)0.0037 (11)
C220.0498 (18)0.0371 (15)0.0375 (15)0.0169 (14)0.0044 (13)0.0055 (12)
C230.058 (2)0.0521 (19)0.0391 (17)0.0216 (16)0.0036 (15)0.0119 (14)
C240.0527 (19)0.0401 (17)0.054 (2)0.0134 (15)0.0036 (15)0.0193 (14)
C250.065 (2)0.0313 (15)0.060 (2)0.0200 (15)0.0031 (17)0.0113 (14)
C260.0543 (19)0.0382 (16)0.0452 (17)0.0242 (14)0.0016 (14)0.0092 (13)
C270.0343 (14)0.0320 (13)0.0353 (14)0.0148 (11)0.0072 (11)0.0072 (11)
C280.0301 (13)0.0273 (12)0.0367 (14)0.0097 (10)0.0068 (11)0.0023 (10)
C290.0440 (16)0.0327 (14)0.0321 (14)0.0107 (12)0.0028 (12)0.0003 (11)
C300.0372 (14)0.0317 (13)0.0321 (14)0.0104 (11)0.0009 (11)0.0049 (11)
C310.0488 (18)0.0333 (15)0.0428 (17)0.0045 (13)0.0041 (14)0.0046 (13)
C320.0494 (19)0.0462 (18)0.0455 (18)0.0010 (15)0.0036 (15)0.0138 (15)
C330.0408 (17)0.0367 (16)0.060 (2)0.0028 (13)0.0121 (15)0.0167 (15)
C340.051 (2)0.0316 (16)0.070 (2)0.0027 (14)0.0001 (17)0.0056 (15)
C350.0440 (17)0.0323 (15)0.0508 (18)0.0076 (13)0.0027 (14)0.0048 (13)
C360.0283 (13)0.0295 (13)0.0407 (15)0.0078 (10)0.0082 (11)0.0059 (11)
Cl10.0507 (4)0.0331 (3)0.0354 (4)0.0136 (3)0.0111 (3)0.0069 (3)
C370.102 (4)0.085 (4)0.062 (3)0.049 (3)0.016 (3)0.012 (2)
Cl20.1090 (15)0.0695 (9)0.0775 (12)0.0381 (10)0.0095 (9)0.0158 (7)
Cl30.0829 (10)0.0906 (11)0.1222 (13)0.0272 (8)0.0125 (9)0.0421 (10)
Cl40.197 (2)0.1644 (19)0.0677 (10)0.1351 (19)0.0021 (11)0.0006 (10)
C37'0.17 (2)0.13 (2)0.10 (2)0.05 (2)0.03 (2)0.01 (2)
Cl2'0.1090 (15)0.0695 (9)0.0775 (12)0.0381 (10)0.0095 (9)0.0158 (7)
Cl3'0.0829 (10)0.0906 (11)0.1222 (13)0.0272 (8)0.0125 (9)0.0421 (10)
Cl4'0.197 (2)0.1644 (19)0.0677 (10)0.1351 (19)0.0021 (11)0.0006 (10)
Geometric parameters (Å, º) top
Ni—N32.052 (2)C13—C181.385 (4)
Ni—N52.054 (2)C13—C141.397 (4)
Ni—N82.075 (2)C14—C151.366 (6)
Ni—N12.121 (2)C15—C161.353 (6)
Ni—Cl12.3091 (8)C16—C171.405 (5)
B1—N41.541 (4)C17—C181.386 (4)
B1—N21.544 (4)C19—C201.390 (4)
B1—N61.549 (4)C19—C271.482 (4)
N1—C11.343 (3)C20—C211.369 (4)
N1—N21.372 (3)C22—C271.382 (4)
N2—C31.341 (4)C22—C231.390 (5)
N3—C101.348 (3)C23—C241.377 (5)
N3—N41.364 (3)C24—C251.376 (5)
N4—C121.348 (3)C25—C261.385 (5)
N5—C191.348 (3)C26—C271.388 (4)
N5—N61.363 (3)C28—C291.381 (4)
N6—C211.339 (3)C28—C361.465 (4)
N7—N81.347 (3)C29—C301.390 (4)
N7—C281.350 (3)C31—C321.384 (4)
N8—C301.325 (4)C31—C361.389 (4)
C1—C21.403 (4)C32—C331.382 (5)
C1—C91.476 (4)C33—C341.386 (5)
C2—C31.370 (4)C34—C351.388 (4)
C4—C51.390 (4)C35—C361.390 (4)
C4—C91.391 (4)C37—Cl41.732 (6)
C5—C61.389 (5)C37—Cl21.768 (6)
C6—C71.378 (5)C37—Cl31.794 (6)
C7—C81.381 (4)C37'—Cl2'1.781 (16)
C8—C91.396 (4)C37'—Cl4'1.787 (16)
C10—C111.402 (4)C37'—Cl3'1.788 (16)
C10—C181.475 (4)Cl3'—Cl3'i1.53 (2)
C11—C121.374 (4)
N3—Ni—N593.84 (9)C8—C9—C1120.7 (3)
N3—Ni—N888.24 (9)N3—C10—C11109.6 (2)
N5—Ni—N888.83 (9)N3—C10—C18121.7 (2)
N3—Ni—N183.78 (9)C11—C10—C18128.6 (2)
N5—Ni—N190.71 (9)C12—C11—C10105.1 (2)
N8—Ni—N1171.96 (9)N4—C12—C11109.0 (2)
N3—Ni—Cl1148.92 (7)C18—C13—C14120.7 (3)
N5—Ni—Cl1117.14 (7)C15—C14—C13120.1 (4)
N8—Ni—Cl189.93 (7)C16—C15—C14120.0 (3)
N1—Ni—Cl197.41 (6)C15—C16—C17120.9 (3)
N4—B1—N2108.7 (2)C18—C17—C16119.8 (3)
N4—B1—N6108.6 (2)C13—C18—C17118.4 (3)
N2—B1—N6108.0 (2)C13—C18—C10121.1 (3)
C1—N1—N2106.2 (2)C17—C18—C10120.3 (3)
C1—N1—Ni140.09 (18)N5—C19—C20109.6 (2)
N2—N1—Ni112.69 (16)N5—C19—C27123.3 (2)
C3—N2—N1109.8 (2)C20—C19—C27127.2 (2)
C3—N2—B1128.5 (2)C21—C20—C19105.7 (2)
N1—N2—B1121.6 (2)N6—C21—C20108.4 (3)
C10—N3—N4106.9 (2)C27—C22—C23119.8 (3)
C10—N3—Ni136.64 (18)C24—C23—C22120.8 (3)
N4—N3—Ni116.05 (16)C25—C24—C23119.5 (3)
C12—N4—N3109.3 (2)C24—C25—C26120.2 (3)
C12—N4—B1130.8 (2)C25—C26—C27120.4 (3)
N3—N4—B1119.8 (2)C22—C27—C26119.3 (3)
C19—N5—N6106.3 (2)C22—C27—C19121.0 (3)
C19—N5—Ni136.12 (18)C26—C27—C19119.7 (3)
N6—N5—Ni116.31 (16)N7—C28—C29105.8 (2)
C21—N6—N5109.9 (2)N7—C28—C36123.5 (3)
C21—N6—B1130.3 (2)C29—C28—C36130.7 (3)
N5—N6—B1119.7 (2)C28—C29—C30105.5 (2)
N8—N7—C28112.3 (2)N8—C30—C29111.2 (3)
C30—N8—N7105.1 (2)C32—C31—C36121.3 (3)
C30—N8—Ni130.41 (19)C33—C32—C31119.5 (3)
N7—N8—Ni123.52 (17)C32—C33—C34120.3 (3)
N1—C1—C2110.0 (2)C33—C34—C35119.6 (3)
N1—C1—C9123.5 (2)C34—C35—C36121.0 (3)
C2—C1—C9126.5 (2)C31—C36—C35118.3 (3)
C3—C2—C1105.2 (3)C31—C36—C28122.9 (3)
N2—C3—C2108.8 (2)C35—C36—C28118.8 (3)
C5—C4—C9120.7 (3)Cl4—C37—Cl2111.5 (3)
C4—C5—C6119.7 (3)Cl4—C37—Cl3108.4 (3)
C7—C6—C5119.9 (3)Cl2—C37—Cl3107.9 (3)
C6—C7—C8120.7 (3)Cl2'—C37'—Cl4'106.1 (13)
C7—C8—C9120.2 (3)Cl2'—C37'—Cl3'109.4 (14)
C4—C9—C8118.8 (3)Cl4'—C37'—Cl3'106.1 (13)
C4—C9—C1120.3 (2)Cl3'i—Cl3'—C37'133.0 (14)
C1—N1—N2—C31.4 (3)C10—C11—C12—N40.4 (3)
Ni—N1—N2—C3169.30 (18)C18—C13—C14—C150.9 (6)
C1—N1—N2—B1177.2 (2)C13—C14—C15—C160.5 (6)
Ni—N1—N2—B112.0 (3)C14—C15—C16—C170.1 (7)
N4—B1—N2—C3128.0 (3)C15—C16—C17—C180.2 (6)
N6—B1—N2—C3114.4 (3)C14—C13—C18—C170.9 (5)
N4—B1—N2—N150.5 (3)C14—C13—C18—C10176.6 (3)
N6—B1—N2—N167.2 (3)C16—C17—C18—C130.6 (5)
C10—N3—N4—C121.2 (3)C16—C17—C18—C10176.3 (3)
Ni—N3—N4—C12172.93 (17)N3—C10—C18—C1328.4 (4)
C10—N3—N4—B1175.5 (2)C11—C10—C18—C13146.1 (3)
Ni—N3—N4—B110.3 (3)N3—C10—C18—C17156.1 (3)
N2—B1—N4—C12123.6 (3)C11—C10—C18—C1729.4 (4)
N6—B1—N4—C12119.1 (3)N6—N5—C19—C200.4 (3)
N2—B1—N4—N352.3 (3)Ni—N5—C19—C20166.5 (2)
N6—B1—N4—N364.9 (3)N6—N5—C19—C27179.1 (2)
C19—N5—N6—C210.7 (3)Ni—N5—C19—C2714.8 (4)
Ni—N5—N6—C21170.02 (18)N5—C19—C20—C210.1 (3)
C19—N5—N6—B1176.2 (2)C27—C19—C20—C21178.6 (3)
Ni—N5—N6—B16.9 (3)N5—N6—C21—C200.7 (3)
N4—B1—N6—C21113.5 (3)B1—N6—C21—C20175.7 (3)
N2—B1—N6—C21128.8 (3)C19—C20—C21—N60.5 (3)
N4—B1—N6—N562.6 (3)C27—C22—C23—C241.0 (5)
N2—B1—N6—N555.1 (3)C22—C23—C24—C250.6 (6)
C28—N7—N8—C300.2 (3)C23—C24—C25—C260.3 (6)
C28—N7—N8—Ni169.62 (18)C24—C25—C26—C270.9 (5)
N2—N1—C1—C21.7 (3)C23—C22—C27—C260.4 (5)
Ni—N1—C1—C2165.0 (2)C23—C22—C27—C19178.0 (3)
N2—N1—C1—C9174.3 (2)C25—C26—C27—C220.5 (5)
Ni—N1—C1—C919.1 (4)C25—C26—C27—C19179.0 (3)
N1—C1—C2—C31.3 (3)N5—C19—C27—C2251.7 (4)
C9—C1—C2—C3174.6 (3)C20—C19—C27—C22126.7 (3)
N1—N2—C3—C20.7 (3)N5—C19—C27—C26129.9 (3)
B1—N2—C3—C2177.9 (3)C20—C19—C27—C2651.7 (4)
C1—C2—C3—N20.3 (3)N8—N7—C28—C290.3 (3)
C9—C4—C5—C60.9 (5)N8—N7—C28—C36179.5 (2)
C4—C5—C6—C70.8 (5)N7—C28—C29—C300.3 (3)
C5—C6—C7—C81.0 (5)C36—C28—C29—C30179.5 (3)
C6—C7—C8—C90.5 (5)N7—N8—C30—C290.0 (3)
C5—C4—C9—C82.3 (4)Ni—N8—C30—C29168.8 (2)
C5—C4—C9—C1178.5 (3)C28—C29—C30—N80.2 (3)
C7—C8—C9—C42.1 (4)C36—C31—C32—C330.8 (6)
C7—C8—C9—C1178.3 (3)C31—C32—C33—C340.2 (6)
N1—C1—C9—C446.0 (4)C32—C33—C34—C351.0 (6)
C2—C1—C9—C4129.3 (3)C33—C34—C35—C360.9 (6)
N1—C1—C9—C8137.9 (3)C32—C31—C36—C350.9 (5)
C2—C1—C9—C846.8 (4)C32—C31—C36—C28179.6 (3)
N4—N3—C10—C111.5 (3)C34—C35—C36—C310.1 (5)
Ni—N3—C10—C11170.8 (2)C34—C35—C36—C28179.6 (3)
N4—N3—C10—C18174.0 (2)N7—C28—C36—C310.4 (4)
Ni—N3—C10—C1813.7 (4)C29—C28—C36—C31179.9 (3)
N3—C10—C11—C121.2 (3)N7—C28—C36—C35179.1 (3)
C18—C10—C11—C12173.9 (3)C29—C28—C36—C350.6 (5)
N3—N4—C12—C110.5 (3)Cl2'—C37'—Cl3'—Cl3'i175.2 (15)
B1—N4—C12—C11175.8 (3)Cl4'—C37'—Cl3'—Cl3'i71 (2)
Symmetry code: (i) x+1, y, z+1.
(cpd3) [Hydrotris(3-phenylpyrazolyl-κN2)borato](phenolato-κO)nickel(II) top
Crystal data top
[Ni(C27H22BN6)(C6H5O)]Z = 2
Mr = 593.12F(000) = 616
Triclinic, P1Dx = 1.360 Mg m3
a = 8.505 (5) ÅMo Kα radiation, λ = 0.71073 Å
b = 13.071 (8) ÅCell parameters from 934 reflections
c = 13.531 (8) Åθ = 1.6–25.2°
α = 79.484 (9)°µ = 0.71 mm1
β = 78.356 (6)°T = 200 K
γ = 87.112 (9)°Plate, brown
V = 1448.4 (15) Å30.40 × 0.26 × 0.12 mm
Data collection top
Bruker APEX
diffractometer
6452 reflections with I > 2σ(I)
Detector resolution: 836.6 pixels mm-1Rint = 0.033
ω scansθmax = 28.3°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1111
Tmin = 0.765, Tmax = 0.920k = 1717
19340 measured reflectionsl = 1817
7128 independent reflections
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)] = 0.068Hydrogen site location: mixed
wR(F2) = 0.205H atoms treated by a mixture of independent and constrained refinement
S = 1.07 w = 1/[σ2(Fo2) + (0.047P)2 + 7.1069P]
where P = (Fo2 + 2Fc2)/3
7128 reflections(Δ/σ)max < 0.001
383 parametersΔρmax = 1.52 e Å3
0 restraintsΔρmin = 0.46 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Refinement. Refined as a 2-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.42651 (7)0.22827 (4)0.16075 (4)0.03231 (16)
B10.5081 (7)0.2703 (4)0.0715 (4)0.0422 (12)
H10.534 (7)0.280 (4)0.155 (4)0.051*
O10.3992 (4)0.2202 (3)0.2989 (2)0.0419 (7)
N10.3594 (5)0.1367 (3)0.0714 (3)0.0377 (8)
N20.4049 (5)0.1720 (3)0.0314 (3)0.0412 (9)
N30.6509 (5)0.2283 (3)0.0770 (3)0.0369 (8)
N40.6595 (5)0.2548 (3)0.0266 (3)0.0406 (9)
N50.3571 (5)0.3583 (3)0.0720 (3)0.0360 (8)
N60.4080 (5)0.3611 (3)0.0305 (3)0.0377 (8)
C10.2745 (6)0.0504 (3)0.0825 (4)0.0397 (10)
C20.2632 (7)0.0295 (4)0.0127 (4)0.0479 (12)
H2A0.20930.02660.02650.058*
C30.3473 (7)0.1079 (4)0.0831 (4)0.0470 (12)
H3A0.36210.11540.15560.056*
C40.3064 (7)0.0302 (4)0.2601 (4)0.0513 (12)
H4A0.40040.00940.25170.062*
C50.2600 (9)0.1016 (5)0.3493 (5)0.0637 (16)
H5A0.32270.11160.40100.076*
C60.1208 (9)0.1589 (5)0.3627 (5)0.0701 (19)
H6A0.08810.20820.42360.084*
C70.0329 (9)0.1436 (5)0.2883 (6)0.074 (2)
H7A0.06160.18280.29760.089*
C80.0772 (7)0.0725 (5)0.1994 (5)0.0561 (14)
H8A0.01180.06210.14900.067*
C90.2183 (6)0.0154 (4)0.1828 (4)0.0419 (11)
C100.8023 (6)0.2160 (3)0.0931 (4)0.0382 (10)
C110.9096 (6)0.2370 (4)0.0003 (4)0.0487 (12)
H11A1.02350.23500.01150.058*
C120.8149 (6)0.2614 (4)0.0734 (4)0.0471 (12)
H12A0.85330.27980.14520.057*
C130.7470 (6)0.1024 (4)0.2639 (4)0.0471 (11)
H13A0.65850.07430.24520.056*
C140.7843 (8)0.0661 (5)0.3598 (5)0.0630 (16)
H14A0.72120.01380.40690.076*
C150.9137 (9)0.1069 (7)0.3856 (5)0.075 (2)
H15A0.94010.08190.45080.090*
C161.0060 (8)0.1839 (6)0.3176 (6)0.0698 (19)
H16A1.09470.21170.33610.084*
C170.9677 (6)0.2198 (5)0.2227 (5)0.0561 (14)
H17A1.03040.27260.17580.067*
C180.8383 (5)0.1793 (4)0.1955 (4)0.0400 (10)
C190.2628 (5)0.4433 (3)0.0818 (4)0.0364 (9)
C200.2533 (6)0.4996 (4)0.0150 (4)0.0437 (11)
H20A0.19430.56220.03030.052*
C210.3470 (6)0.4456 (4)0.0832 (4)0.0416 (10)
H21A0.36570.46480.15570.050*
C220.2636 (7)0.4624 (4)0.2623 (4)0.0464 (11)
H22A0.36830.43230.25690.056*
C230.1889 (8)0.4968 (5)0.3519 (4)0.0567 (14)
H23A0.24360.49070.40740.068*
C240.0353 (8)0.5399 (5)0.3609 (5)0.0615 (16)
H24A0.01410.56470.42180.074*
C250.0440 (8)0.5466 (5)0.2822 (5)0.0614 (16)
H25A0.15000.57470.28920.074*
C260.0274 (6)0.5129 (4)0.1916 (4)0.0495 (12)
H26A0.03010.51730.13750.059*
C270.1843 (5)0.4724 (3)0.1805 (4)0.0369 (9)
C280.5723 (6)0.3200 (4)0.3632 (4)0.0452 (11)
H28A0.63590.33970.29670.054*
C290.6103 (7)0.3557 (5)0.4442 (5)0.0575 (14)
H29A0.70080.39910.43300.069*
C300.5207 (9)0.3301 (6)0.5413 (5)0.0695 (18)
H30A0.54740.35610.59690.083*
C310.3906 (8)0.2657 (6)0.5565 (5)0.0686 (18)
H31A0.32760.24660.62340.082*
C320.3518 (7)0.2289 (5)0.4750 (4)0.0503 (12)
H32A0.26190.18490.48660.060*
C330.4418 (5)0.2553 (3)0.3765 (3)0.0366 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0349 (3)0.0309 (3)0.0314 (3)0.0005 (2)0.0048 (2)0.0082 (2)
B10.053 (3)0.039 (3)0.033 (2)0.004 (2)0.004 (2)0.011 (2)
O10.0434 (18)0.0489 (19)0.0339 (16)0.0047 (15)0.0065 (14)0.0089 (14)
N10.042 (2)0.0335 (18)0.0386 (19)0.0006 (15)0.0064 (16)0.0097 (15)
N20.054 (2)0.0345 (19)0.037 (2)0.0009 (17)0.0101 (17)0.0124 (16)
N30.0380 (19)0.0342 (18)0.0383 (19)0.0007 (15)0.0044 (16)0.0092 (15)
N40.045 (2)0.0344 (19)0.039 (2)0.0019 (16)0.0000 (17)0.0084 (16)
N50.041 (2)0.0328 (18)0.0347 (18)0.0008 (15)0.0060 (15)0.0095 (15)
N60.047 (2)0.0342 (19)0.0339 (18)0.0031 (16)0.0102 (16)0.0083 (15)
C10.038 (2)0.031 (2)0.053 (3)0.0038 (17)0.010 (2)0.0159 (19)
C20.052 (3)0.040 (3)0.059 (3)0.002 (2)0.017 (2)0.024 (2)
C30.059 (3)0.043 (3)0.045 (3)0.008 (2)0.016 (2)0.022 (2)
C40.046 (3)0.047 (3)0.057 (3)0.003 (2)0.005 (2)0.004 (2)
C50.074 (4)0.055 (3)0.055 (3)0.001 (3)0.002 (3)0.004 (3)
C60.087 (5)0.050 (3)0.061 (4)0.013 (3)0.017 (4)0.012 (3)
C70.068 (4)0.065 (4)0.082 (5)0.031 (3)0.028 (4)0.034 (4)
C80.044 (3)0.059 (3)0.069 (4)0.013 (2)0.003 (3)0.033 (3)
C90.036 (2)0.032 (2)0.057 (3)0.0013 (18)0.001 (2)0.019 (2)
C100.037 (2)0.0269 (19)0.049 (3)0.0020 (16)0.0034 (19)0.0096 (18)
C110.040 (3)0.037 (2)0.062 (3)0.002 (2)0.007 (2)0.010 (2)
C120.051 (3)0.037 (2)0.046 (3)0.004 (2)0.009 (2)0.009 (2)
C130.045 (3)0.041 (3)0.055 (3)0.003 (2)0.014 (2)0.006 (2)
C140.066 (4)0.062 (4)0.057 (3)0.015 (3)0.008 (3)0.007 (3)
C150.070 (4)0.107 (6)0.058 (4)0.042 (4)0.028 (3)0.034 (4)
C160.044 (3)0.101 (5)0.077 (4)0.013 (3)0.023 (3)0.039 (4)
C170.035 (2)0.065 (4)0.074 (4)0.001 (2)0.009 (2)0.028 (3)
C180.033 (2)0.037 (2)0.053 (3)0.0062 (17)0.0082 (19)0.015 (2)
C190.039 (2)0.031 (2)0.042 (2)0.0014 (17)0.0104 (18)0.0095 (17)
C200.053 (3)0.035 (2)0.044 (3)0.004 (2)0.013 (2)0.0069 (19)
C210.053 (3)0.034 (2)0.038 (2)0.002 (2)0.011 (2)0.0039 (18)
C220.052 (3)0.041 (3)0.046 (3)0.000 (2)0.008 (2)0.008 (2)
C230.067 (4)0.062 (3)0.042 (3)0.002 (3)0.006 (3)0.015 (3)
C240.076 (4)0.052 (3)0.046 (3)0.006 (3)0.011 (3)0.010 (2)
C250.060 (3)0.052 (3)0.063 (4)0.009 (3)0.009 (3)0.010 (3)
C260.042 (3)0.048 (3)0.057 (3)0.005 (2)0.006 (2)0.011 (2)
C270.037 (2)0.035 (2)0.040 (2)0.0030 (17)0.0053 (18)0.0117 (18)
C280.040 (2)0.043 (3)0.051 (3)0.004 (2)0.003 (2)0.009 (2)
C290.053 (3)0.055 (3)0.069 (4)0.011 (3)0.023 (3)0.009 (3)
C300.088 (5)0.078 (4)0.054 (3)0.013 (4)0.030 (3)0.020 (3)
C310.070 (4)0.100 (5)0.037 (3)0.018 (4)0.007 (3)0.014 (3)
C320.045 (3)0.066 (3)0.039 (3)0.013 (2)0.006 (2)0.008 (2)
C330.036 (2)0.035 (2)0.038 (2)0.0008 (17)0.0081 (18)0.0056 (18)
Geometric parameters (Å, º) top
Ni1—O11.820 (3)C8—C91.403 (7)
Ni1—N32.013 (4)C10—C111.393 (7)
Ni1—N12.023 (4)C10—C181.468 (7)
Ni1—N52.030 (4)C11—C121.381 (8)
B1—N41.521 (7)C13—C181.386 (7)
B1—N21.544 (7)C13—C141.391 (8)
B1—N61.545 (7)C14—C151.379 (10)
O1—C331.339 (5)C15—C161.388 (11)
N1—C11.339 (6)C16—C171.382 (9)
N1—N21.366 (5)C17—C181.385 (7)
N2—C31.350 (6)C19—C201.395 (7)
N3—C101.345 (6)C19—C271.474 (6)
N3—N41.368 (5)C20—C211.366 (7)
N4—C121.345 (6)C22—C231.391 (7)
N5—C191.347 (6)C22—C271.392 (7)
N5—N61.362 (5)C23—C241.388 (9)
N6—C211.343 (6)C24—C251.359 (10)
C1—C21.387 (7)C25—C261.392 (8)
C1—C91.472 (7)C26—C271.400 (7)
C2—C31.383 (8)C28—C291.368 (8)
C4—C51.384 (8)C28—C331.391 (7)
C4—C91.386 (8)C29—C301.370 (9)
C5—C61.396 (10)C30—C311.383 (9)
C6—C71.352 (11)C31—C321.384 (8)
C7—C81.378 (10)C32—C331.389 (7)
O1—Ni1—N3119.00 (16)C4—C9—C8117.8 (5)
O1—Ni1—N1133.29 (16)C4—C9—C1122.4 (4)
N3—Ni1—N188.94 (16)C8—C9—C1119.6 (5)
O1—Ni1—N5120.34 (16)N3—C10—C11109.5 (5)
N3—Ni1—N593.93 (16)N3—C10—C18122.3 (4)
N1—Ni1—N591.27 (16)C11—C10—C18128.2 (5)
N4—B1—N2108.5 (4)C12—C11—C10105.2 (5)
N4—B1—N6109.0 (4)N4—C12—C11109.1 (5)
N2—B1—N6106.5 (4)C18—C13—C14120.2 (5)
C33—O1—Ni1147.1 (3)C15—C14—C13119.3 (6)
C1—N1—N2106.9 (4)C14—C15—C16120.8 (6)
C1—N1—Ni1138.6 (3)C17—C16—C15119.5 (6)
N2—N1—Ni1114.4 (3)C16—C17—C18120.3 (6)
C3—N2—N1109.2 (4)C17—C18—C13119.8 (5)
C3—N2—B1130.3 (4)C17—C18—C10119.7 (5)
N1—N2—B1120.5 (4)C13—C18—C10120.5 (4)
C10—N3—N4107.4 (4)N5—C19—C20109.8 (4)
C10—N3—Ni1138.1 (3)N5—C19—C27124.6 (4)
N4—N3—Ni1114.3 (3)C20—C19—C27125.6 (4)
C12—N4—N3108.8 (4)C21—C20—C19105.4 (4)
C12—N4—B1130.2 (4)N6—C21—C20108.6 (4)
N3—N4—B1121.0 (4)C23—C22—C27119.7 (5)
C19—N5—N6106.2 (4)C24—C23—C22120.6 (6)
C19—N5—Ni1139.5 (3)C25—C24—C23119.6 (5)
N6—N5—Ni1114.1 (3)C24—C25—C26121.2 (6)
C21—N6—N5110.0 (4)C25—C26—C27119.6 (6)
C21—N6—B1128.9 (4)C22—C27—C26119.2 (5)
N5—N6—B1120.9 (4)C22—C27—C19121.5 (4)
N1—C1—C2110.3 (5)C26—C27—C19119.3 (4)
N1—C1—C9122.7 (4)C29—C28—C33121.1 (5)
C2—C1—C9126.8 (4)C28—C29—C30121.4 (5)
C3—C2—C1105.2 (4)C29—C30—C31118.6 (5)
N2—C3—C2108.4 (5)C30—C31—C32120.4 (6)
C5—C4—C9121.2 (6)C31—C32—C33121.1 (5)
C4—C5—C6119.7 (7)O1—C33—C32119.7 (4)
C7—C6—C5119.4 (6)O1—C33—C28122.9 (4)
C6—C7—C8121.6 (6)C32—C33—C28117.4 (5)
C7—C8—C9120.3 (6)
N3—Ni1—O1—C3347.1 (6)N4—N3—C10—C18175.2 (4)
N1—Ni1—O1—C33166.7 (5)Ni1—N3—C10—C1810.2 (7)
N5—Ni1—O1—C3367.4 (6)N3—C10—C11—C120.7 (5)
C1—N1—N2—C30.4 (5)C18—C10—C11—C12175.6 (4)
Ni1—N1—N2—C3177.1 (3)N3—N4—C12—C111.2 (5)
C1—N1—N2—B1178.9 (4)B1—N4—C12—C11177.8 (5)
Ni1—N1—N2—B13.6 (5)C10—C11—C12—N40.3 (6)
N4—B1—N2—C3123.7 (5)C18—C13—C14—C150.5 (9)
N6—B1—N2—C3119.2 (5)C13—C14—C15—C160.5 (10)
N4—B1—N2—N155.5 (5)C14—C15—C16—C170.2 (10)
N6—B1—N2—N161.6 (6)C15—C16—C17—C180.0 (9)
C10—N3—N4—C121.6 (5)C16—C17—C18—C130.0 (8)
Ni1—N3—N4—C12174.5 (3)C16—C17—C18—C10178.1 (5)
C10—N3—N4—B1177.5 (4)C14—C13—C18—C170.3 (8)
Ni1—N3—N4—B16.4 (5)C14—C13—C18—C10178.3 (5)
N2—B1—N4—C12125.0 (5)N3—C10—C18—C17143.3 (5)
N6—B1—N4—C12119.4 (5)C11—C10—C18—C1740.8 (7)
N2—B1—N4—N353.8 (5)N3—C10—C18—C1338.7 (7)
N6—B1—N4—N361.8 (5)C11—C10—C18—C13137.2 (5)
C19—N5—N6—C210.1 (5)N6—N5—C19—C200.3 (5)
Ni1—N5—N6—C21175.4 (3)Ni1—N5—C19—C20173.2 (4)
C19—N5—N6—B1174.8 (4)N6—N5—C19—C27178.8 (4)
Ni1—N5—N6—B10.5 (5)Ni1—N5—C19—C277.7 (8)
N4—B1—N6—C21128.3 (5)N5—C19—C20—C210.6 (6)
N2—B1—N6—C21114.9 (5)C27—C19—C20—C21178.5 (4)
N4—B1—N6—N557.9 (6)N5—N6—C21—C200.4 (6)
N2—B1—N6—N559.0 (6)B1—N6—C21—C20174.0 (5)
N2—N1—C1—C20.5 (5)C19—C20—C21—N60.6 (6)
Ni1—N1—C1—C2176.0 (4)C27—C22—C23—C240.7 (9)
N2—N1—C1—C9173.9 (4)C22—C23—C24—C251.4 (9)
Ni1—N1—C1—C99.6 (8)C23—C24—C25—C261.4 (10)
N1—C1—C2—C30.4 (6)C24—C25—C26—C270.7 (9)
C9—C1—C2—C3173.7 (5)C23—C22—C27—C262.7 (8)
N1—N2—C3—C20.2 (6)C23—C22—C27—C19176.0 (5)
B1—N2—C3—C2179.1 (5)C25—C26—C27—C222.8 (8)
C1—C2—C3—N20.1 (6)C25—C26—C27—C19176.0 (5)
C9—C4—C5—C61.0 (9)N5—C19—C27—C2241.0 (7)
C4—C5—C6—C70.1 (10)C20—C19—C27—C22137.9 (5)
C5—C6—C7—C80.1 (10)N5—C19—C27—C26140.3 (5)
C6—C7—C8—C91.5 (9)C20—C19—C27—C2640.8 (7)
C5—C4—C9—C82.3 (8)C33—C28—C29—C300.7 (9)
C5—C4—C9—C1172.6 (5)C28—C29—C30—C310.8 (11)
C7—C8—C9—C42.5 (8)C29—C30—C31—C320.5 (12)
C7—C8—C9—C1172.5 (5)C30—C31—C32—C330.1 (11)
N1—C1—C9—C434.5 (7)Ni1—O1—C33—C32168.4 (5)
C2—C1—C9—C4139.0 (5)Ni1—O1—C33—C2810.2 (9)
N1—C1—C9—C8150.8 (5)C31—C32—C33—O1178.7 (6)
C2—C1—C9—C835.7 (7)C31—C32—C33—C280.0 (9)
N4—N3—C10—C111.4 (5)C29—C28—C33—O1178.9 (5)
Ni1—N3—C10—C11173.2 (4)C29—C28—C33—C320.3 (8)
Calculated τ values for (2), (3), (4), (5) and (6) top
(2)0.38a
(3)0.75b, 0.71c
(4)0.75b, 0.75c 0.76b, 0.73c
(5)0.74b, 0.70c
(6)0.27a
References: (a) τ5 (Addison et al., 1984); (b) τ4 (Yang et al., 2007); (c) τ'4 (Okuniewski et al., 2015).
 

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