Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270113017022/yp3036sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270113017022/yp30361sup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270113017022/yp30362sup3.hkl |
CCDC references: 964747; 964748
For both compounds, data collection: APEX2 (Bruker, 2009); cell refinement: SAINT (Bruker, 2009); data reduction: SAINT (Bruker, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEP-3 (Farrugia, 2012). Software used to prepare material for publication: WinGX (Farrugia, 20120) for (1); WinGX (Farrugia, 2012) for (2).
[Co(C27H38BN6)(N3)] | Z = 4 |
Mr = 558.40 | F(000) = 1180 |
Monoclinic, P21/n | Dx = 1.308 Mg m−3 |
a = 9.8910 (3) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 17.7415 (5) Å | µ = 0.64 mm−1 |
c = 16.1660 (5) Å | T = 223 K |
β = 92.016 (2)° | Plate, blue |
V = 2835.07 (15) Å3 | 0.17 × 0.07 × 0.05 mm |
Bruker APEXII CCD area-detector diffractometer | 7050 independent reflections |
Radiation source: fine-focus sealed tube | 4482 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.086 |
phi and ω scans | θmax = 28.3°, θmin = 2.6° |
Absorption correction: multi-scan (APEX2; Bruker, 2009) | h = −13→12 |
Tmin = 0.675, Tmax = 0.746 | k = −23→23 |
50578 measured reflections | l = −21→21 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0427P)2 + 0.921P] where P = (Fo2 + 2Fc2)/3 |
7050 reflections | (Δ/σ)max = 0.002 |
361 parameters | Δρmax = 0.31 e Å−3 |
0 restraints | Δρmin = −0.32 e Å−3 |
[Co(C27H38BN6)(N3)] | V = 2835.07 (15) Å3 |
Mr = 558.40 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 9.8910 (3) Å | µ = 0.64 mm−1 |
b = 17.7415 (5) Å | T = 223 K |
c = 16.1660 (5) Å | 0.17 × 0.07 × 0.05 mm |
β = 92.016 (2)° |
Bruker APEXII CCD area-detector diffractometer | 7050 independent reflections |
Absorption correction: multi-scan (APEX2; Bruker, 2009) | 4482 reflections with I > 2σ(I) |
Tmin = 0.675, Tmax = 0.746 | Rint = 0.086 |
50578 measured reflections |
R[F2 > 2σ(F2)] = 0.043 | 0 restraints |
wR(F2) = 0.107 | H-atom parameters constrained |
S = 1.01 | Δρmax = 0.31 e Å−3 |
7050 reflections | Δρmin = −0.32 e Å−3 |
361 parameters |
Experimental. The quality of the glove-box atmosphere was periodically checked with a toluene solution of 'titanocene' (Watt et al., 1966). Glassware was dried at 423 K overnight. Diethyl ether, pentane, tetrahydrofuran (THF) and toluene were purified using the Glass Contour solvent purification system. Deuterated benzene was dried first over CaH2, then over Na/benzophenone, before vacuum transfer into a storage container. Before use, aliquots of Et2O, THF and toluene were tested with a drop of Na/benzophenone in THF solution. 1H NMR data were recorded on a Varian Unity 400 spectrometer (400 MHz) at 295 K. All resonances in the 1H NMR spectra are referenced to residual C6D5H (δ 7.16 p.p.m.). IR spectra were recorded on a Thermo Scientific Nicolet iS10 SMART iTR spectrophotometer. Watt, G. W., Baye, L. D. & Drummond, F. O. (1966). J. Am. Chem. Soc. 88, 1138–1140. |
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Co1 | 0.53081 (3) | 0.281366 (17) | 0.923847 (18) | 0.02599 (10) | |
B1 | 0.3498 (3) | 0.14526 (14) | 0.94792 (15) | 0.0249 (5) | |
N1 | 0.6491 (3) | 0.36786 (13) | 0.91310 (14) | 0.0567 (7) | |
N2 | 0.7069 (3) | 0.40560 (14) | 0.86969 (16) | 0.0587 (7) | |
N3A | 0.7950 (13) | 0.4334 (9) | 0.8389 (11) | 0.118 (6) | 0.50 |
N3B | 0.7312 (14) | 0.4542 (7) | 0.8198 (8) | 0.097 (5) | 0.50 |
N11 | 0.44370 (18) | 0.15999 (10) | 1.02720 (10) | 0.0241 (4) | |
N12 | 0.59306 (18) | 0.21796 (10) | 1.10630 (10) | 0.0249 (4) | |
C11 | 0.5364 (2) | 0.21725 (12) | 1.02858 (13) | 0.0252 (5) | |
C12 | 0.4417 (2) | 0.12730 (13) | 1.10507 (13) | 0.0275 (5) | |
H12 | 0.3855 | 0.0875 | 1.1209 | 0.033* | |
C13 | 0.5342 (2) | 0.16252 (13) | 1.15372 (13) | 0.0297 (5) | |
H13 | 0.5553 | 0.1517 | 1.2096 | 0.036* | |
C14 | 0.6974 (2) | 0.27364 (13) | 1.13612 (14) | 0.0304 (5) | |
C15 | 0.6302 (3) | 0.35045 (14) | 1.14288 (18) | 0.0449 (7) | |
H15A | 0.5946 | 0.3658 | 1.0888 | 0.067* | |
H15B | 0.6963 | 0.3871 | 1.1630 | 0.067* | |
H15C | 0.5570 | 0.3474 | 1.1811 | 0.067* | |
C16 | 0.7536 (3) | 0.24987 (17) | 1.22019 (15) | 0.0462 (7) | |
H16A | 0.6813 | 0.2492 | 1.2592 | 0.069* | |
H16B | 0.8228 | 0.2853 | 1.2389 | 0.069* | |
H16C | 0.7927 | 0.1999 | 1.2164 | 0.069* | |
C17 | 0.8104 (3) | 0.27707 (15) | 1.07513 (16) | 0.0406 (6) | |
H17A | 0.7738 | 0.2927 | 1.0214 | 0.061* | |
H17B | 0.8514 | 0.2277 | 1.0705 | 0.061* | |
H17C | 0.8782 | 0.3131 | 1.0945 | 0.061* | |
N21 | 0.26605 (18) | 0.22091 (10) | 0.93681 (10) | 0.0244 (4) | |
N22 | 0.2248 (2) | 0.34016 (11) | 0.92153 (12) | 0.0325 (5) | |
C21 | 0.3259 (2) | 0.28846 (12) | 0.92296 (13) | 0.0270 (5) | |
C22 | 0.1289 (2) | 0.23182 (13) | 0.94674 (14) | 0.0325 (5) | |
H22 | 0.0653 | 0.1943 | 0.9585 | 0.039* | |
C23 | 0.1031 (3) | 0.30579 (14) | 0.93647 (15) | 0.0368 (6) | |
H23 | 0.0183 | 0.3295 | 0.9390 | 0.044* | |
C24 | 0.2462 (3) | 0.42341 (13) | 0.90890 (16) | 0.0409 (6) | |
C25 | 0.3329 (4) | 0.45248 (16) | 0.97996 (18) | 0.0759 (12) | |
H25A | 0.2849 | 0.4472 | 1.0309 | 0.114* | |
H25B | 0.3536 | 0.5052 | 0.9709 | 0.114* | |
H25C | 0.4164 | 0.4238 | 0.9840 | 0.114* | |
C26 | 0.1103 (4) | 0.46268 (19) | 0.9048 (3) | 0.0916 (14) | |
H26A | 0.0534 | 0.4401 | 0.8614 | 0.137* | |
H26B | 0.1231 | 0.5157 | 0.8930 | 0.137* | |
H26C | 0.0672 | 0.4573 | 0.9575 | 0.137* | |
C27 | 0.3148 (4) | 0.43462 (15) | 0.82745 (17) | 0.0569 (9) | |
H27A | 0.2555 | 0.4172 | 0.7824 | 0.085* | |
H27B | 0.3985 | 0.4061 | 0.8279 | 0.085* | |
H27C | 0.3344 | 0.4877 | 0.8199 | 0.085* | |
N31 | 0.44609 (18) | 0.13749 (10) | 0.87232 (10) | 0.0234 (4) | |
N32 | 0.59785 (18) | 0.16278 (11) | 0.78303 (11) | 0.0291 (4) | |
C31 | 0.5341 (2) | 0.19142 (13) | 0.84874 (13) | 0.0261 (5) | |
C32 | 0.4577 (2) | 0.07508 (13) | 0.82140 (14) | 0.0314 (5) | |
H32 | 0.4083 | 0.0300 | 0.8249 | 0.038* | |
C33 | 0.5520 (3) | 0.09049 (14) | 0.76632 (15) | 0.0372 (6) | |
H33 | 0.5813 | 0.0583 | 0.7244 | 0.045* | |
C34 | 0.7049 (2) | 0.20494 (15) | 0.73852 (14) | 0.0356 (6) | |
C35 | 0.8251 (3) | 0.21573 (17) | 0.79946 (16) | 0.0470 (7) | |
H35A | 0.7972 | 0.2457 | 0.8461 | 0.070* | |
H35B | 0.8975 | 0.2414 | 0.7720 | 0.070* | |
H35C | 0.8568 | 0.1669 | 0.8190 | 0.070* | |
C36 | 0.6468 (3) | 0.28044 (16) | 0.70991 (16) | 0.0442 (6) | |
H36A | 0.6157 | 0.3082 | 0.7573 | 0.066* | |
H36B | 0.5715 | 0.2719 | 0.6710 | 0.066* | |
H36C | 0.7163 | 0.3093 | 0.6832 | 0.066* | |
C37 | 0.7463 (3) | 0.15995 (18) | 0.66382 (16) | 0.0521 (8) | |
H37A | 0.7865 | 0.1126 | 0.6820 | 0.078* | |
H37B | 0.8117 | 0.1885 | 0.6333 | 0.078* | |
H37C | 0.6673 | 0.1499 | 0.6283 | 0.078* | |
C41 | 0.2559 (2) | 0.07130 (12) | 0.94747 (14) | 0.0271 (5) | |
C42 | 0.1457 (2) | 0.06672 (14) | 0.89043 (15) | 0.0348 (6) | |
H42 | 0.1237 | 0.1091 | 0.8578 | 0.042* | |
C43 | 0.0687 (3) | 0.00237 (16) | 0.88061 (18) | 0.0463 (7) | |
H43 | −0.0051 | 0.0018 | 0.8424 | 0.056* | |
C44 | 0.0993 (3) | −0.06083 (16) | 0.92643 (19) | 0.0514 (8) | |
H44 | 0.0456 | −0.1043 | 0.9208 | 0.062* | |
C45 | 0.2100 (3) | −0.05984 (15) | 0.98099 (18) | 0.0486 (7) | |
H45 | 0.2331 | −0.1034 | 1.0115 | 0.058* | |
C46 | 0.2869 (3) | 0.00484 (13) | 0.99094 (15) | 0.0360 (6) | |
H46 | 0.3623 | 0.0042 | 1.0280 | 0.043* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.03306 (18) | 0.02144 (15) | 0.02341 (15) | −0.00589 (14) | 0.00026 (12) | 0.00168 (13) |
B1 | 0.0266 (14) | 0.0212 (12) | 0.0268 (13) | 0.0011 (11) | 0.0002 (10) | 0.0010 (10) |
N1 | 0.0839 (19) | 0.0401 (14) | 0.0464 (14) | −0.0355 (13) | 0.0068 (13) | 0.0017 (11) |
N2 | 0.0706 (19) | 0.0429 (15) | 0.0634 (17) | −0.0262 (14) | 0.0149 (14) | −0.0060 (13) |
N3A | 0.101 (9) | 0.087 (10) | 0.170 (15) | −0.050 (7) | 0.072 (9) | −0.005 (8) |
N3B | 0.164 (14) | 0.060 (6) | 0.070 (5) | −0.053 (8) | 0.032 (8) | 0.018 (4) |
N11 | 0.0267 (10) | 0.0210 (9) | 0.0246 (9) | −0.0016 (8) | 0.0014 (8) | 0.0024 (7) |
N12 | 0.0275 (10) | 0.0239 (9) | 0.0231 (9) | −0.0002 (8) | −0.0014 (7) | −0.0001 (8) |
C11 | 0.0276 (12) | 0.0223 (11) | 0.0257 (11) | 0.0002 (10) | −0.0004 (9) | 0.0001 (9) |
C12 | 0.0338 (13) | 0.0246 (11) | 0.0242 (11) | −0.0014 (10) | 0.0037 (10) | 0.0036 (9) |
C13 | 0.0371 (14) | 0.0300 (12) | 0.0219 (11) | −0.0001 (11) | 0.0010 (10) | 0.0056 (9) |
C14 | 0.0324 (13) | 0.0312 (13) | 0.0269 (11) | −0.0052 (11) | −0.0059 (10) | −0.0026 (10) |
C15 | 0.0472 (17) | 0.0303 (14) | 0.0570 (17) | −0.0042 (12) | −0.0018 (13) | −0.0079 (12) |
C16 | 0.0468 (17) | 0.0571 (17) | 0.0334 (14) | −0.0159 (14) | −0.0167 (12) | 0.0030 (13) |
C17 | 0.0324 (14) | 0.0498 (16) | 0.0394 (14) | −0.0071 (13) | 0.0011 (11) | −0.0020 (12) |
N21 | 0.0269 (10) | 0.0223 (9) | 0.0240 (9) | −0.0005 (8) | 0.0010 (7) | 0.0020 (8) |
N22 | 0.0421 (13) | 0.0244 (10) | 0.0312 (11) | 0.0068 (9) | 0.0030 (9) | 0.0009 (8) |
C21 | 0.0352 (13) | 0.0226 (11) | 0.0233 (10) | 0.0027 (10) | 0.0008 (9) | −0.0003 (9) |
C22 | 0.0262 (13) | 0.0355 (14) | 0.0358 (13) | 0.0019 (10) | 0.0029 (10) | 0.0003 (10) |
C23 | 0.0332 (14) | 0.0385 (14) | 0.0389 (14) | 0.0085 (12) | 0.0030 (11) | −0.0012 (11) |
C24 | 0.0642 (19) | 0.0204 (12) | 0.0384 (14) | 0.0086 (12) | 0.0031 (13) | 0.0013 (10) |
C25 | 0.155 (4) | 0.0267 (15) | 0.0447 (18) | −0.0160 (19) | −0.013 (2) | −0.0031 (13) |
C26 | 0.095 (3) | 0.0387 (19) | 0.143 (4) | 0.033 (2) | 0.029 (3) | 0.022 (2) |
C27 | 0.102 (3) | 0.0250 (14) | 0.0444 (16) | 0.0000 (15) | 0.0069 (17) | 0.0061 (12) |
N31 | 0.0250 (10) | 0.0215 (9) | 0.0238 (9) | −0.0008 (8) | 0.0006 (8) | −0.0009 (7) |
N32 | 0.0269 (11) | 0.0337 (11) | 0.0268 (10) | −0.0021 (9) | 0.0029 (8) | −0.0029 (8) |
C31 | 0.0257 (12) | 0.0288 (12) | 0.0237 (11) | −0.0018 (10) | −0.0014 (9) | −0.0003 (9) |
C32 | 0.0356 (14) | 0.0226 (12) | 0.0360 (13) | −0.0017 (10) | 0.0021 (11) | −0.0071 (10) |
C33 | 0.0385 (15) | 0.0364 (14) | 0.0368 (14) | −0.0005 (12) | 0.0035 (11) | −0.0130 (11) |
C34 | 0.0266 (13) | 0.0514 (17) | 0.0292 (12) | −0.0068 (12) | 0.0051 (10) | −0.0008 (11) |
C35 | 0.0271 (14) | 0.070 (2) | 0.0437 (15) | −0.0112 (14) | −0.0004 (11) | 0.0032 (14) |
C36 | 0.0394 (15) | 0.0539 (17) | 0.0395 (14) | −0.0085 (14) | 0.0066 (12) | 0.0119 (13) |
C37 | 0.0437 (17) | 0.077 (2) | 0.0366 (15) | −0.0056 (16) | 0.0120 (13) | −0.0094 (14) |
C41 | 0.0264 (12) | 0.0243 (12) | 0.0308 (12) | −0.0039 (10) | 0.0051 (10) | −0.0028 (9) |
C42 | 0.0327 (14) | 0.0290 (13) | 0.0425 (14) | −0.0027 (11) | −0.0012 (11) | −0.0019 (11) |
C43 | 0.0360 (16) | 0.0440 (16) | 0.0585 (18) | −0.0080 (13) | −0.0040 (13) | −0.0153 (14) |
C44 | 0.0505 (18) | 0.0332 (15) | 0.071 (2) | −0.0189 (14) | 0.0131 (16) | −0.0130 (14) |
C45 | 0.066 (2) | 0.0238 (13) | 0.0567 (18) | −0.0064 (13) | 0.0121 (16) | 0.0014 (12) |
C46 | 0.0425 (15) | 0.0251 (12) | 0.0405 (14) | −0.0022 (11) | 0.0019 (12) | −0.0003 (11) |
Co1—N1 | 1.941 (2) | C24—C27 | 1.516 (4) |
Co1—C11 | 2.039 (2) | C25—H25A | 0.9700 |
Co1—C21 | 2.030 (2) | C25—H25B | 0.9700 |
Co1—C31 | 2.006 (2) | C25—H25C | 0.9700 |
B1—N11 | 1.578 (3) | C26—H26A | 0.9700 |
B1—N31 | 1.582 (3) | C26—H26B | 0.9700 |
B1—N21 | 1.584 (3) | C26—H26C | 0.9700 |
B1—C41 | 1.607 (3) | C27—H27A | 0.9700 |
N1—N2 | 1.138 (3) | C27—H27B | 0.9700 |
N2—N3A | 1.132 (13) | C27—H27C | 0.9700 |
N2—N3B | 1.211 (11) | N31—C31 | 1.357 (3) |
N3A—N3B | 0.786 (19) | N31—C32 | 1.387 (3) |
N11—C11 | 1.368 (3) | N32—C31 | 1.353 (3) |
N11—C12 | 1.387 (3) | N32—C33 | 1.384 (3) |
N12—C11 | 1.358 (3) | N32—C34 | 1.501 (3) |
N12—C13 | 1.388 (3) | C32—C33 | 1.340 (3) |
N12—C14 | 1.496 (3) | C32—H32 | 0.9400 |
C12—C13 | 1.340 (3) | C33—H33 | 0.9400 |
C12—H12 | 0.9400 | C34—C37 | 1.516 (3) |
C13—H13 | 0.9400 | C34—C36 | 1.523 (4) |
C14—C16 | 1.510 (3) | C34—C35 | 1.528 (3) |
C14—C17 | 1.517 (3) | C35—H35A | 0.9700 |
C14—C15 | 1.522 (3) | C35—H35B | 0.9700 |
C15—H15A | 0.9700 | C35—H35C | 0.9700 |
C15—H15B | 0.9700 | C36—H36A | 0.9700 |
C15—H15C | 0.9700 | C36—H36B | 0.9700 |
C16—H16A | 0.9700 | C36—H36C | 0.9700 |
C16—H16B | 0.9700 | C37—H37A | 0.9700 |
C16—H16C | 0.9700 | C37—H37B | 0.9700 |
C17—H17A | 0.9700 | C37—H37C | 0.9700 |
C17—H17B | 0.9700 | C41—C46 | 1.401 (3) |
C17—H17C | 0.9700 | C41—C42 | 1.405 (3) |
N21—C21 | 1.359 (3) | C42—C43 | 1.379 (3) |
N21—C22 | 1.385 (3) | C42—H42 | 0.9400 |
N22—C21 | 1.357 (3) | C43—C44 | 1.372 (4) |
N22—C23 | 1.379 (3) | C43—H43 | 0.9400 |
N22—C24 | 1.507 (3) | C44—C45 | 1.381 (4) |
C22—C23 | 1.346 (3) | C44—H44 | 0.9400 |
C22—H22 | 0.9400 | C45—C46 | 1.383 (4) |
C23—H23 | 0.9400 | C45—H45 | 0.9400 |
C24—C25 | 1.501 (4) | C46—H46 | 0.9400 |
C24—C26 | 1.513 (4) | ||
N1—Co1—C31 | 123.50 (10) | C26—C24—C27 | 109.0 (3) |
N1—Co1—C21 | 123.72 (11) | C24—C25—H25A | 109.5 |
N1—Co1—C11 | 121.10 (10) | C24—C25—H25B | 109.5 |
C11—Co1—C21 | 92.20 (9) | H25A—C25—H25B | 109.5 |
C11—Co1—C31 | 93.34 (9) | C24—C25—H25C | 109.5 |
C21—Co1—C31 | 94.73 (9) | H25A—C25—H25C | 109.5 |
N11—B1—N31 | 106.77 (18) | H25B—C25—H25C | 109.5 |
N11—B1—N21 | 104.02 (17) | C24—C26—H26A | 109.5 |
N31—B1—N21 | 108.24 (17) | C24—C26—H26B | 109.5 |
N11—B1—C41 | 117.54 (18) | H26A—C26—H26B | 109.5 |
N31—B1—C41 | 106.80 (17) | C24—C26—H26C | 109.5 |
N21—B1—C41 | 113.05 (19) | H26A—C26—H26C | 109.5 |
N2—N1—Co1 | 146.9 (2) | H26B—C26—H26C | 109.5 |
N3A—N2—N1 | 159.8 (8) | C24—C27—H27A | 109.5 |
N1—N2—N3B | 161.0 (7) | C24—C27—H27B | 109.5 |
N3B—N3A—N2 | 75.9 (17) | H27A—C27—H27B | 109.5 |
N3A—N3B—N2 | 65.1 (15) | C24—C27—H27C | 109.5 |
C11—N11—C12 | 109.06 (18) | H27A—C27—H27C | 109.5 |
C11—N11—B1 | 120.75 (17) | H27B—C27—H27C | 109.5 |
C12—N11—B1 | 129.88 (18) | C31—N31—C32 | 109.20 (18) |
C11—N12—C13 | 109.71 (18) | C31—N31—B1 | 124.41 (18) |
C11—N12—C14 | 124.19 (18) | C32—N31—B1 | 126.37 (18) |
C13—N12—C14 | 126.01 (18) | C31—N32—C33 | 110.02 (19) |
N12—C11—N11 | 106.05 (18) | C31—N32—C34 | 123.06 (19) |
N12—C11—Co1 | 139.60 (17) | C33—N32—C34 | 126.90 (19) |
N11—C11—Co1 | 113.71 (14) | N32—C31—N31 | 106.08 (18) |
C13—C12—N11 | 107.85 (19) | N32—C31—Co1 | 142.33 (17) |
C13—C12—H12 | 126.1 | N31—C31—Co1 | 111.51 (14) |
N11—C12—H12 | 126.1 | C33—C32—N31 | 107.8 (2) |
C12—C13—N12 | 107.29 (19) | C33—C32—H32 | 126.1 |
C12—C13—H13 | 126.4 | N31—C32—H32 | 126.1 |
N12—C13—H13 | 126.4 | C32—C33—N32 | 106.9 (2) |
N12—C14—C16 | 109.47 (19) | C32—C33—H33 | 126.6 |
N12—C14—C17 | 109.42 (18) | N32—C33—H33 | 126.6 |
C16—C14—C17 | 109.9 (2) | N32—C34—C37 | 109.5 (2) |
N12—C14—C15 | 108.42 (19) | N32—C34—C36 | 108.58 (19) |
C16—C14—C15 | 109.5 (2) | C37—C34—C36 | 109.3 (2) |
C17—C14—C15 | 110.1 (2) | N32—C34—C35 | 107.40 (19) |
C14—C15—H15A | 109.5 | C37—C34—C35 | 110.7 (2) |
C14—C15—H15B | 109.5 | C36—C34—C35 | 111.2 (2) |
H15A—C15—H15B | 109.5 | C34—C35—H35A | 109.5 |
C14—C15—H15C | 109.5 | C34—C35—H35B | 109.5 |
H15A—C15—H15C | 109.5 | H35A—C35—H35B | 109.5 |
H15B—C15—H15C | 109.5 | C34—C35—H35C | 109.5 |
C14—C16—H16A | 109.5 | H35A—C35—H35C | 109.5 |
C14—C16—H16B | 109.5 | H35B—C35—H35C | 109.5 |
H16A—C16—H16B | 109.5 | C34—C36—H36A | 109.5 |
C14—C16—H16C | 109.5 | C34—C36—H36B | 109.5 |
H16A—C16—H16C | 109.5 | H36A—C36—H36B | 109.5 |
H16B—C16—H16C | 109.5 | C34—C36—H36C | 109.5 |
C14—C17—H17A | 109.5 | H36A—C36—H36C | 109.5 |
C14—C17—H17B | 109.5 | H36B—C36—H36C | 109.5 |
H17A—C17—H17B | 109.5 | C34—C37—H37A | 109.5 |
C14—C17—H17C | 109.5 | C34—C37—H37B | 109.5 |
H17A—C17—H17C | 109.5 | H37A—C37—H37B | 109.5 |
H17B—C17—H17C | 109.5 | C34—C37—H37C | 109.5 |
C21—N21—C22 | 109.27 (18) | H37A—C37—H37C | 109.5 |
C21—N21—B1 | 122.47 (18) | H37B—C37—H37C | 109.5 |
C22—N21—B1 | 127.99 (18) | C46—C41—C42 | 115.6 (2) |
C21—N22—C23 | 110.23 (19) | C46—C41—B1 | 124.7 (2) |
C21—N22—C24 | 123.9 (2) | C42—C41—B1 | 119.0 (2) |
C23—N22—C24 | 125.8 (2) | C43—C42—C41 | 122.4 (2) |
N22—C21—N21 | 105.89 (19) | C43—C42—H42 | 118.8 |
N22—C21—Co1 | 141.01 (17) | C41—C42—H42 | 118.8 |
N21—C21—Co1 | 112.64 (15) | C44—C43—C42 | 120.3 (3) |
C23—C22—N21 | 107.8 (2) | C44—C43—H43 | 119.9 |
C23—C22—H22 | 126.1 | C42—C43—H43 | 119.9 |
N21—C22—H22 | 126.1 | C43—C44—C45 | 119.3 (3) |
C22—C23—N22 | 106.8 (2) | C43—C44—H44 | 120.3 |
C22—C23—H23 | 126.6 | C45—C44—H44 | 120.3 |
N22—C23—H23 | 126.6 | C44—C45—C46 | 120.3 (3) |
C25—C24—N22 | 108.2 (2) | C44—C45—H45 | 119.8 |
C25—C24—C26 | 111.0 (3) | C46—C45—H45 | 119.8 |
N22—C24—C26 | 109.2 (2) | C45—C46—C41 | 122.0 (3) |
C25—C24—C27 | 111.0 (3) | C45—C46—H46 | 119.0 |
N22—C24—C27 | 108.40 (19) | C41—C46—H46 | 119.0 |
[Co(C27H38BN6)(N3)2] | V = 1495.2 (4) Å3 |
Mr = 600.43 | Z = 2 |
Triclinic, P1 | F(000) = 632 |
a = 10.1553 (14) Å | Dx = 1.334 Mg m−3 |
b = 12.3593 (18) Å | Mo Kα radiation, λ = 0.71073 Å |
c = 12.8113 (17) Å | µ = 0.61 mm−1 |
α = 82.350 (9)° | T = 228 K |
β = 69.88 (1)° | Needle, green |
γ = 85.26 (1)° | 0.28 × 0.05 × 0.02 mm |
Bruker APEXII CCD area detector diffractometer | 6113 independent reflections |
Radiation source: fine-focus sealed tube | 3105 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.126 |
phi and ω scans | θmax = 26.4°, θmin = 1.7° |
Absorption correction: multi-scan (APEX2; Bruker, 2009) | h = −12→12 |
Tmin = 0.621, Tmax = 0.745 | k = −14→15 |
24620 measured reflections | l = −16→16 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.060 | H-atom parameters constrained |
wR(F2) = 0.143 | w = 1/[σ2(Fo2) + (0.0624P)2] where P = (Fo2 + 2Fc2)/3 |
S = 0.92 | (Δ/σ)max < 0.001 |
6113 reflections | Δρmax = 0.34 e Å−3 |
380 parameters | Δρmin = −0.45 e Å−3 |
0 restraints | Extinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0133 (15) |
[Co(C27H38BN6)(N3)2] | γ = 85.26 (1)° |
Mr = 600.43 | V = 1495.2 (4) Å3 |
Triclinic, P1 | Z = 2 |
a = 10.1553 (14) Å | Mo Kα radiation |
b = 12.3593 (18) Å | µ = 0.61 mm−1 |
c = 12.8113 (17) Å | T = 228 K |
α = 82.350 (9)° | 0.28 × 0.05 × 0.02 mm |
β = 69.88 (1)° |
Bruker APEXII CCD area detector diffractometer | 6113 independent reflections |
Absorption correction: multi-scan (APEX2; Bruker, 2009) | 3105 reflections with I > 2σ(I) |
Tmin = 0.621, Tmax = 0.745 | Rint = 0.126 |
24620 measured reflections |
R[F2 > 2σ(F2)] = 0.060 | 0 restraints |
wR(F2) = 0.143 | H-atom parameters constrained |
S = 0.92 | Δρmax = 0.34 e Å−3 |
6113 reflections | Δρmin = −0.45 e Å−3 |
380 parameters |
Geometry. All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. |
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > 2σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Co1 | 0.61577 (6) | 0.71224 (4) | 0.74346 (5) | 0.0273 (2) | |
B1 | 0.8509 (5) | 0.7760 (4) | 0.5191 (4) | 0.0270 (11) | |
N1 | 0.7886 (3) | 0.6659 (3) | 0.5218 (3) | 0.0273 (8) | |
N2 | 0.6777 (4) | 0.5199 (3) | 0.6140 (3) | 0.0303 (9) | |
N3 | 0.7265 (3) | 0.8611 (2) | 0.5551 (3) | 0.0245 (8) | |
N4 | 0.5485 (3) | 0.9484 (3) | 0.6666 (3) | 0.0265 (8) | |
N5 | 0.9055 (3) | 0.7576 (3) | 0.6212 (3) | 0.0284 (8) | |
N6 | 0.9031 (4) | 0.7128 (3) | 0.7920 (3) | 0.0321 (9) | |
N7 | 0.5310 (4) | 0.7339 (3) | 0.8990 (3) | 0.0380 (9) | |
N8 | 0.4082 (5) | 0.7190 (3) | 0.9532 (3) | 0.0392 (10) | |
N9 | 0.2927 (5) | 0.7046 (4) | 1.0088 (3) | 0.0620 (13) | |
N10 | 0.4292 (4) | 0.6898 (3) | 0.7359 (3) | 0.0323 (9) | |
N11 | 0.4102 (4) | 0.7093 (3) | 0.6477 (3) | 0.0310 (9) | |
N12 | 0.3842 (4) | 0.7269 (3) | 0.5657 (3) | 0.0463 (11) | |
C1 | 0.6930 (4) | 0.6277 (3) | 0.6206 (3) | 0.0279 (10) | |
C2 | 0.8345 (5) | 0.5819 (4) | 0.4542 (4) | 0.0367 (11) | |
H2 | 0.9025 | 0.5865 | 0.3823 | 0.044* | |
C3 | 0.7643 (5) | 0.4931 (4) | 0.5100 (4) | 0.0391 (12) | |
H3 | 0.7723 | 0.4248 | 0.4834 | 0.047* | |
C4 | 0.5925 (5) | 0.4366 (3) | 0.7020 (4) | 0.0327 (11) | |
C5 | 0.6754 (5) | 0.3275 (3) | 0.6926 (4) | 0.0473 (13) | |
H5A | 0.6840 | 0.3011 | 0.6224 | 0.071* | |
H5B | 0.6267 | 0.2749 | 0.7544 | 0.071* | |
H5C | 0.7681 | 0.3372 | 0.6949 | 0.071* | |
C6 | 0.4545 (5) | 0.4263 (4) | 0.6819 (4) | 0.0453 (13) | |
H6A | 0.4020 | 0.4957 | 0.6888 | 0.068* | |
H6B | 0.3997 | 0.3707 | 0.7367 | 0.068* | |
H6C | 0.4741 | 0.4058 | 0.6073 | 0.068* | |
C7 | 0.5685 (5) | 0.4707 (4) | 0.8158 (4) | 0.0501 (13) | |
H7A | 0.6582 | 0.4802 | 0.8240 | 0.075* | |
H7B | 0.5182 | 0.4149 | 0.8730 | 0.075* | |
H7C | 0.5137 | 0.5391 | 0.8238 | 0.075* | |
C8 | 0.6243 (4) | 0.8495 (3) | 0.6563 (3) | 0.0256 (10) | |
C9 | 0.7179 (4) | 0.9647 (3) | 0.5033 (3) | 0.0280 (10) | |
H9 | 0.7782 | 0.9932 | 0.4329 | 0.034* | |
C10 | 0.6086 (4) | 1.0179 (3) | 0.5708 (3) | 0.0312 (10) | |
H10 | 0.5778 | 1.0902 | 0.5556 | 0.037* | |
C11 | 0.4300 (4) | 0.9892 (3) | 0.7657 (3) | 0.0319 (10) | |
C12 | 0.3854 (5) | 1.1058 (3) | 0.7302 (4) | 0.0382 (11) | |
H12A | 0.3576 | 1.1061 | 0.6649 | 0.057* | |
H12B | 0.4634 | 1.1533 | 0.7123 | 0.057* | |
H12C | 0.3069 | 1.1317 | 0.7909 | 0.057* | |
C13 | 0.4849 (5) | 0.9925 (4) | 0.8612 (3) | 0.0394 (12) | |
H13A | 0.4110 | 1.0199 | 0.9240 | 0.059* | |
H13B | 0.5636 | 1.0403 | 0.8370 | 0.059* | |
H13C | 0.5155 | 0.9194 | 0.8838 | 0.059* | |
C14 | 0.3022 (4) | 0.9187 (3) | 0.7979 (4) | 0.0368 (11) | |
H14A | 0.2706 | 0.9206 | 0.7342 | 0.055* | |
H14B | 0.2273 | 0.9467 | 0.8597 | 0.055* | |
H14C | 0.3275 | 0.8439 | 0.8200 | 0.055* | |
C15 | 0.8173 (4) | 0.7294 (3) | 0.7275 (3) | 0.0271 (10) | |
C16 | 1.0415 (4) | 0.7568 (3) | 0.6200 (4) | 0.0346 (11) | |
H16 | 1.1212 | 0.7721 | 0.5566 | 0.042* | |
C17 | 1.0406 (5) | 0.7305 (4) | 0.7242 (4) | 0.0384 (11) | |
H17 | 1.1192 | 0.7248 | 0.7477 | 0.046* | |
C18 | 0.8651 (5) | 0.6843 (4) | 0.9164 (4) | 0.0338 (11) | |
C19 | 0.7801 (5) | 0.5821 (4) | 0.9520 (4) | 0.0449 (13) | |
H19A | 0.6913 | 0.5975 | 0.9393 | 0.067* | |
H19B | 0.7628 | 0.5595 | 1.0309 | 0.067* | |
H19C | 0.8318 | 0.5242 | 0.9087 | 0.067* | |
C20 | 0.9976 (5) | 0.6609 (4) | 0.9470 (4) | 0.0531 (14) | |
H20A | 1.0533 | 0.6023 | 0.9067 | 0.080* | |
H20B | 0.9721 | 0.6392 | 1.0269 | 0.080* | |
H20C | 1.0519 | 0.7261 | 0.9271 | 0.080* | |
C21 | 0.7854 (5) | 0.7804 (4) | 0.9749 (4) | 0.0474 (13) | |
H21A | 0.8454 | 0.8425 | 0.9536 | 0.071* | |
H21B | 0.7569 | 0.7611 | 1.0552 | 0.071* | |
H21C | 0.7030 | 0.7991 | 0.9534 | 0.071* | |
C22 | 0.9599 (4) | 0.8224 (3) | 0.4000 (3) | 0.0290 (10) | |
C23 | 0.9484 (4) | 0.8003 (3) | 0.3002 (3) | 0.0347 (11) | |
H23 | 0.8808 | 0.7515 | 0.3026 | 0.042* | |
C24 | 1.0327 (5) | 0.8475 (4) | 0.1970 (4) | 0.0441 (12) | |
H24 | 1.0250 | 0.8276 | 0.1311 | 0.053* | |
C25 | 1.1269 (5) | 0.9227 (4) | 0.1908 (4) | 0.0497 (14) | |
H25 | 1.1842 | 0.9547 | 0.1208 | 0.060* | |
C26 | 1.1376 (5) | 0.9515 (4) | 0.2879 (4) | 0.0433 (12) | |
H26 | 1.2002 | 1.0048 | 0.2846 | 0.052* | |
C27 | 1.0555 (4) | 0.9013 (3) | 0.3903 (4) | 0.0354 (11) | |
H27 | 1.0645 | 0.9211 | 0.4558 | 0.043* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Co1 | 0.0211 (3) | 0.0287 (4) | 0.0322 (4) | −0.0001 (2) | −0.0101 (3) | −0.0017 (3) |
B1 | 0.021 (3) | 0.027 (3) | 0.033 (3) | −0.001 (2) | −0.009 (2) | −0.007 (2) |
N1 | 0.0208 (19) | 0.026 (2) | 0.035 (2) | 0.0021 (15) | −0.0079 (16) | −0.0063 (17) |
N2 | 0.029 (2) | 0.025 (2) | 0.037 (2) | −0.0018 (16) | −0.0107 (18) | −0.0055 (17) |
N3 | 0.0235 (19) | 0.025 (2) | 0.027 (2) | −0.0015 (15) | −0.0115 (16) | −0.0014 (15) |
N4 | 0.0203 (19) | 0.028 (2) | 0.032 (2) | 0.0025 (15) | −0.0096 (16) | −0.0057 (16) |
N5 | 0.0192 (19) | 0.032 (2) | 0.035 (2) | −0.0005 (15) | −0.0104 (17) | −0.0054 (16) |
N6 | 0.023 (2) | 0.038 (2) | 0.037 (2) | −0.0008 (16) | −0.0130 (18) | −0.0042 (17) |
N7 | 0.027 (2) | 0.051 (2) | 0.037 (2) | 0.0024 (18) | −0.0114 (19) | −0.0081 (18) |
N8 | 0.041 (3) | 0.045 (3) | 0.030 (2) | 0.010 (2) | −0.014 (2) | −0.0005 (19) |
N9 | 0.037 (3) | 0.090 (4) | 0.047 (3) | 0.008 (2) | −0.005 (2) | 0.007 (2) |
N10 | 0.026 (2) | 0.032 (2) | 0.039 (2) | −0.0003 (16) | −0.0134 (18) | 0.0008 (18) |
N11 | 0.023 (2) | 0.024 (2) | 0.045 (3) | −0.0014 (15) | −0.010 (2) | −0.0028 (18) |
N12 | 0.047 (3) | 0.053 (3) | 0.046 (3) | −0.002 (2) | −0.026 (2) | −0.002 (2) |
C1 | 0.024 (2) | 0.029 (3) | 0.036 (3) | 0.0022 (19) | −0.019 (2) | −0.001 (2) |
C2 | 0.037 (3) | 0.036 (3) | 0.035 (3) | 0.002 (2) | −0.007 (2) | −0.012 (2) |
C3 | 0.044 (3) | 0.028 (3) | 0.046 (3) | 0.001 (2) | −0.013 (2) | −0.014 (2) |
C4 | 0.032 (3) | 0.024 (2) | 0.042 (3) | −0.0058 (19) | −0.014 (2) | 0.001 (2) |
C5 | 0.046 (3) | 0.029 (3) | 0.064 (3) | 0.003 (2) | −0.019 (3) | 0.001 (2) |
C6 | 0.040 (3) | 0.036 (3) | 0.062 (3) | −0.008 (2) | −0.022 (3) | 0.002 (2) |
C7 | 0.059 (4) | 0.044 (3) | 0.048 (3) | −0.008 (3) | −0.021 (3) | 0.004 (2) |
C8 | 0.022 (2) | 0.029 (3) | 0.028 (2) | −0.0001 (19) | −0.0101 (19) | −0.0062 (19) |
C9 | 0.028 (2) | 0.031 (3) | 0.026 (2) | −0.005 (2) | −0.010 (2) | −0.002 (2) |
C10 | 0.032 (3) | 0.027 (2) | 0.036 (3) | −0.005 (2) | −0.014 (2) | 0.001 (2) |
C11 | 0.026 (2) | 0.035 (3) | 0.037 (3) | 0.006 (2) | −0.012 (2) | −0.013 (2) |
C12 | 0.036 (3) | 0.028 (3) | 0.051 (3) | 0.004 (2) | −0.016 (2) | −0.008 (2) |
C13 | 0.035 (3) | 0.050 (3) | 0.034 (3) | 0.007 (2) | −0.012 (2) | −0.013 (2) |
C14 | 0.023 (2) | 0.039 (3) | 0.045 (3) | 0.004 (2) | −0.007 (2) | −0.006 (2) |
C15 | 0.025 (2) | 0.029 (2) | 0.032 (3) | 0.0027 (18) | −0.015 (2) | −0.0040 (19) |
C16 | 0.018 (2) | 0.043 (3) | 0.045 (3) | 0.000 (2) | −0.011 (2) | −0.006 (2) |
C17 | 0.022 (3) | 0.050 (3) | 0.046 (3) | 0.002 (2) | −0.016 (2) | −0.005 (2) |
C18 | 0.029 (3) | 0.042 (3) | 0.035 (3) | 0.004 (2) | −0.019 (2) | −0.002 (2) |
C19 | 0.048 (3) | 0.046 (3) | 0.044 (3) | 0.003 (2) | −0.021 (2) | −0.001 (2) |
C20 | 0.044 (3) | 0.068 (4) | 0.056 (3) | −0.004 (3) | −0.032 (3) | 0.004 (3) |
C21 | 0.054 (3) | 0.047 (3) | 0.048 (3) | 0.006 (3) | −0.025 (3) | −0.012 (3) |
C22 | 0.021 (2) | 0.029 (2) | 0.035 (3) | 0.0010 (19) | −0.006 (2) | −0.007 (2) |
C23 | 0.027 (3) | 0.038 (3) | 0.039 (3) | −0.003 (2) | −0.010 (2) | −0.004 (2) |
C24 | 0.042 (3) | 0.056 (3) | 0.032 (3) | −0.002 (3) | −0.009 (2) | −0.006 (2) |
C25 | 0.042 (3) | 0.053 (3) | 0.043 (3) | −0.011 (3) | −0.003 (3) | 0.008 (3) |
C26 | 0.032 (3) | 0.047 (3) | 0.047 (3) | −0.012 (2) | −0.009 (2) | 0.002 (2) |
C27 | 0.031 (3) | 0.040 (3) | 0.037 (3) | −0.003 (2) | −0.013 (2) | −0.006 (2) |
Co1—C8 | 1.894 (4) | C7—H7C | 0.9700 |
Co1—C1 | 1.907 (4) | C9—C10 | 1.335 (5) |
Co1—N7 | 1.926 (4) | C9—H9 | 0.9400 |
Co1—N10 | 1.974 (4) | C10—H10 | 0.9400 |
Co1—C15 | 2.012 (4) | C11—C13 | 1.515 (6) |
B1—N1 | 1.538 (6) | C11—C14 | 1.529 (6) |
B1—N3 | 1.557 (6) | C11—C12 | 1.532 (5) |
B1—N5 | 1.571 (6) | C12—H12A | 0.9700 |
B1—C22 | 1.610 (6) | C12—H12B | 0.9700 |
N1—C1 | 1.356 (5) | C12—H12C | 0.9700 |
N1—C2 | 1.388 (5) | C13—H13A | 0.9700 |
N2—C1 | 1.371 (5) | C13—H13B | 0.9700 |
N2—C3 | 1.386 (5) | C13—H13C | 0.9700 |
N2—C4 | 1.499 (5) | C14—H14A | 0.9700 |
N3—C8 | 1.352 (5) | C14—H14B | 0.9700 |
N3—C9 | 1.372 (5) | C14—H14C | 0.9700 |
N4—C10 | 1.381 (5) | C16—C17 | 1.328 (6) |
N4—C8 | 1.386 (5) | C16—H16 | 0.9400 |
N4—C11 | 1.528 (5) | C17—H17 | 0.9400 |
N5—C15 | 1.366 (5) | C18—C21 | 1.512 (6) |
N5—C16 | 1.376 (5) | C18—C19 | 1.518 (6) |
N6—C15 | 1.381 (5) | C18—C20 | 1.522 (6) |
N6—C17 | 1.384 (5) | C19—H19A | 0.9700 |
N6—C18 | 1.503 (5) | C19—H19B | 0.9700 |
N7—N8 | 1.216 (5) | C19—H19C | 0.9700 |
N8—N9 | 1.157 (5) | C20—H20A | 0.9700 |
N10—N11 | 1.201 (5) | C20—H20B | 0.9700 |
N11—N12 | 1.158 (5) | C20—H20C | 0.9700 |
C2—C3 | 1.339 (6) | C21—H21A | 0.9700 |
C2—H2 | 0.9400 | C21—H21B | 0.9700 |
C3—H3 | 0.9400 | C21—H21C | 0.9700 |
C4—C7 | 1.506 (6) | C22—C23 | 1.387 (5) |
C4—C5 | 1.525 (6) | C22—C27 | 1.397 (6) |
C4—C6 | 1.528 (6) | C23—C24 | 1.385 (6) |
C5—H5A | 0.9700 | C23—H23 | 0.9400 |
C5—H5B | 0.9700 | C24—C25 | 1.364 (6) |
C5—H5C | 0.9700 | C24—H24 | 0.9400 |
C6—H6A | 0.9700 | C25—C26 | 1.380 (6) |
C6—H6B | 0.9700 | C25—H25 | 0.9400 |
C6—H6C | 0.9700 | C26—C27 | 1.384 (6) |
C7—H7A | 0.9700 | C26—H26 | 0.9400 |
C7—H7B | 0.9700 | C27—H27 | 0.9400 |
C1—Co1—C8 | 96.26 (17) | C9—C10—H10 | 125.8 |
C8—Co1—N7 | 108.63 (16) | N4—C10—H10 | 125.8 |
C1—Co1—N7 | 155.02 (16) | C13—C11—N4 | 108.9 (3) |
C8—Co1—N10 | 90.76 (15) | C13—C11—C14 | 113.1 (4) |
C1—Co1—N10 | 87.37 (16) | N4—C11—C14 | 110.6 (3) |
N7—Co1—N10 | 90.09 (15) | C13—C11—C12 | 108.4 (3) |
C8—Co1—C15 | 87.23 (16) | N4—C11—C12 | 108.3 (3) |
C1—Co1—C15 | 84.57 (17) | C14—C11—C12 | 107.5 (4) |
N7—Co1—C15 | 98.45 (16) | C11—C12—H12A | 109.5 |
N10—Co1—C15 | 171.42 (16) | C11—C12—H12B | 109.5 |
N1—B1—N3 | 107.6 (3) | H12A—C12—H12B | 109.5 |
N1—B1—N5 | 103.4 (3) | C11—C12—H12C | 109.5 |
N3—B1—N5 | 103.6 (3) | H12A—C12—H12C | 109.5 |
N1—B1—C22 | 115.5 (3) | H12B—C12—H12C | 109.5 |
N3—B1—C22 | 108.6 (3) | C11—C13—H13A | 109.5 |
N5—B1—C22 | 117.1 (3) | C11—C13—H13B | 109.5 |
C1—N1—C2 | 109.3 (3) | H13A—C13—H13B | 109.5 |
C1—N1—B1 | 116.1 (3) | C11—C13—H13C | 109.5 |
C2—N1—B1 | 132.2 (3) | H13A—C13—H13C | 109.5 |
C1—N2—C3 | 108.8 (3) | H13B—C13—H13C | 109.5 |
C1—N2—C4 | 129.1 (4) | C11—C14—H14A | 109.5 |
C3—N2—C4 | 122.0 (3) | C11—C14—H14B | 109.5 |
C8—N3—C9 | 109.9 (3) | H14A—C14—H14B | 109.5 |
C8—N3—B1 | 122.4 (3) | C11—C14—H14C | 109.5 |
C9—N3—B1 | 126.5 (3) | H14A—C14—H14C | 109.5 |
C10—N4—C8 | 108.0 (3) | H14B—C14—H14C | 109.5 |
C10—N4—C11 | 120.9 (3) | N5—C15—N6 | 104.9 (3) |
C8—N4—C11 | 130.7 (3) | N5—C15—Co1 | 115.7 (3) |
C15—N5—C16 | 110.0 (3) | N6—C15—Co1 | 139.2 (3) |
C15—N5—B1 | 121.5 (3) | C17—C16—N5 | 108.1 (4) |
C16—N5—B1 | 128.3 (3) | C17—C16—H16 | 126.0 |
C15—N6—C17 | 109.3 (4) | N5—C16—H16 | 126.0 |
C15—N6—C18 | 129.5 (3) | C16—C17—N6 | 107.8 (4) |
C17—N6—C18 | 121.3 (4) | C16—C17—H17 | 126.1 |
N8—N7—Co1 | 124.0 (3) | N6—C17—H17 | 126.1 |
N9—N8—N7 | 177.1 (5) | N6—C18—C21 | 109.2 (3) |
N11—N10—Co1 | 119.2 (3) | N6—C18—C19 | 109.1 (3) |
N12—N11—N10 | 176.2 (5) | C21—C18—C19 | 112.0 (4) |
N1—C1—N2 | 106.4 (3) | N6—C18—C20 | 110.0 (3) |
N1—C1—Co1 | 123.2 (3) | C21—C18—C20 | 108.1 (4) |
N2—C1—Co1 | 130.1 (3) | C19—C18—C20 | 108.3 (4) |
C3—C2—N1 | 107.6 (4) | C18—C19—H19A | 109.5 |
C3—C2—H2 | 126.2 | C18—C19—H19B | 109.5 |
N1—C2—H2 | 126.2 | H19A—C19—H19B | 109.5 |
C2—C3—N2 | 107.9 (4) | C18—C19—H19C | 109.5 |
C2—C3—H3 | 126.1 | H19A—C19—H19C | 109.5 |
N2—C3—H3 | 126.1 | H19B—C19—H19C | 109.5 |
N2—C4—C7 | 109.3 (3) | C18—C20—H20A | 109.5 |
N2—C4—C5 | 108.5 (4) | C18—C20—H20B | 109.5 |
C7—C4—C5 | 108.5 (4) | H20A—C20—H20B | 109.5 |
N2—C4—C6 | 108.6 (3) | C18—C20—H20C | 109.5 |
C7—C4—C6 | 111.8 (4) | H20A—C20—H20C | 109.5 |
C5—C4—C6 | 110.0 (4) | H20B—C20—H20C | 109.5 |
C4—C5—H5A | 109.5 | C18—C21—H21A | 109.5 |
C4—C5—H5B | 109.5 | C18—C21—H21B | 109.5 |
H5A—C5—H5B | 109.5 | H21A—C21—H21B | 109.5 |
C4—C5—H5C | 109.5 | C18—C21—H21C | 109.5 |
H5A—C5—H5C | 109.5 | H21A—C21—H21C | 109.5 |
H5B—C5—H5C | 109.5 | H21B—C21—H21C | 109.5 |
C4—C6—H6A | 109.5 | C23—C22—C27 | 115.6 (4) |
C4—C6—H6B | 109.5 | C23—C22—B1 | 121.5 (4) |
H6A—C6—H6B | 109.5 | C27—C22—B1 | 122.1 (4) |
C4—C6—H6C | 109.5 | C24—C23—C22 | 122.4 (4) |
H6A—C6—H6C | 109.5 | C24—C23—H23 | 118.8 |
H6B—C6—H6C | 109.5 | C22—C23—H23 | 118.8 |
C4—C7—H7A | 109.5 | C25—C24—C23 | 120.2 (4) |
C4—C7—H7B | 109.5 | C25—C24—H24 | 119.9 |
H7A—C7—H7B | 109.5 | C23—C24—H24 | 119.9 |
C4—C7—H7C | 109.5 | C24—C25—C26 | 119.5 (4) |
H7A—C7—H7C | 109.5 | C24—C25—H25 | 120.2 |
H7B—C7—H7C | 109.5 | C26—C25—H25 | 120.2 |
N3—C8—N4 | 106.0 (3) | C25—C26—C27 | 119.6 (4) |
N3—C8—Co1 | 117.3 (3) | C25—C26—H26 | 120.2 |
N4—C8—Co1 | 136.6 (3) | C27—C26—H26 | 120.2 |
C10—C9—N3 | 107.8 (4) | C26—C27—C22 | 122.5 (4) |
C10—C9—H9 | 126.1 | C26—C27—H27 | 118.7 |
N3—C9—H9 | 126.1 | C22—C27—H27 | 118.7 |
C9—C10—N4 | 108.3 (4) |
Experimental details
(1) | (2) | |
Crystal data | ||
Chemical formula | [Co(C27H38BN6)(N3)] | [Co(C27H38BN6)(N3)2] |
Mr | 558.40 | 600.43 |
Crystal system, space group | Monoclinic, P21/n | Triclinic, P1 |
Temperature (K) | 223 | 228 |
a, b, c (Å) | 9.8910 (3), 17.7415 (5), 16.1660 (5) | 10.1553 (14), 12.3593 (18), 12.8113 (17) |
α, β, γ (°) | 90, 92.016 (2), 90 | 82.350 (9), 69.88 (1), 85.26 (1) |
V (Å3) | 2835.07 (15) | 1495.2 (4) |
Z | 4 | 2 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 0.64 | 0.61 |
Crystal size (mm) | 0.17 × 0.07 × 0.05 | 0.28 × 0.05 × 0.02 |
Data collection | ||
Diffractometer | Bruker APEXII CCD area-detector diffractometer | Bruker APEXII CCD area detector diffractometer |
Absorption correction | Multi-scan (APEX2; Bruker, 2009) | Multi-scan (APEX2; Bruker, 2009) |
Tmin, Tmax | 0.675, 0.746 | 0.621, 0.745 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 50578, 7050, 4482 | 24620, 6113, 3105 |
Rint | 0.086 | 0.126 |
(sin θ/λ)max (Å−1) | 0.668 | 0.626 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.107, 1.01 | 0.060, 0.143, 0.92 |
No. of reflections | 7050 | 6113 |
No. of parameters | 361 | 380 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.31, −0.32 | 0.34, −0.45 |
Computer programs: APEX2 (Bruker, 2009), SAINT (Bruker, 2009), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEP-3 (Farrugia, 2012), WinGX (Farrugia, 20120), WinGX (Farrugia, 2012).
Co1—N1 | 1.941 (2) | Co1—C31 | 2.006 (2) |
Co1—C11 | 2.039 (2) | N1—N2 | 1.138 (3) |
Co1—C21 | 2.030 (2) | N2—N3A | 1.132 (13) |
C11—Co1—C21 | 92.20 (9) | N2—N1—Co1 | 146.9 (2) |
C11—Co1—C31 | 93.34 (9) | N3A—N2—N1 | 159.8 (8) |
C21—Co1—C31 | 94.73 (9) |
Co1—C8 | 1.894 (4) | N7—N8 | 1.216 (5) |
Co1—C1 | 1.907 (4) | N8—N9 | 1.157 (5) |
Co1—N7 | 1.926 (4) | N10—N11 | 1.201 (5) |
Co1—N10 | 1.974 (4) | N11—N12 | 1.158 (5) |
Co1—C15 | 2.012 (4) | ||
C1—Co1—C8 | 96.26 (17) | N10—Co1—C15 | 171.42 (16) |
C8—Co1—N7 | 108.63 (16) | N8—N7—Co1 | 124.0 (3) |
C1—Co1—N7 | 155.02 (16) | N9—N8—N7 | 177.1 (5) |
C8—Co1—N10 | 90.76 (15) | N11—N10—Co1 | 119.2 (3) |
C8—Co1—C15 | 87.23 (16) | N12—N11—N10 | 176.2 (5) |
C1—Co1—C15 | 84.57 (17) |
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