Triaceto­nitrile­(1,4,7-trimethyl-1,4,7-tri­aza­cyclonona­ne)cobalt(II) bis­(tetra­phenyl­borate)

The title cobalt(II) complex, [Co(C₂H₃N)₃(C₉H₂₁N₃)](C₂₄H₂₀B)₂ or [(tacn)Co(NCMe)₃][BPh₄]₂, has been characterized by single-crystal X-ray diffraction. It incorporates the well-known macrocyclic tacn (1,4,7-trimethyl-1,4,7-tri­aza­cyclo­nona­ne) ligand, which is coordinated facially to the metal center. The complex crystallizes in space group P2₁/c with Z = 4. The divalent cobalt ion exhibits a six-coordinate octa­hedral geometry by one tacn and three aceto­nitrile ligands. Two non-coordinating tetra­phenyl­borate (BPh₄⁻) anions are also present.

Key indicators

Structure: I

• Single-crystal X-ray study
• T = 133 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.056
• wR factor = 0.107
• Data-to-parameter ratio = 14.4

checkCIF/PLATON results

No syntax errors found



Alert level C
THETM01_ALERT_3_C  The value of sine(theta_max)/wavelength is less than 0.590
            Calculated sin(theta_max)/wavelength =    0.5892
PLAT048_ALERT_1_C MoietyFormula Not Given (or Incomplete) ........     Please Check
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ......      6.737 Check
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.589         24 Report
               16  9  3,  10 12  4,  -6 13  5,   6 13  5,  17  8  5,  -5 13  7,
               18  5 12,  19  3 12,  19  2 13, -19  1 14, -11 10 14, -17  5 15,
               17  4 16,  14  7 17,  15  6 17,  16  4 18,  16  3 19,  16  1 20,
               14  3 22, -11  2 26,   4  6 27,   6  4 28,   3  4 29,   3  2 30,

Alert level G
PLAT432_ALERT_2_G Short Inter X...Y Contact  C12      ..C24      .       3.18 Ang.
                                                      x,y,z  =      1_555 Check
PLAT794_ALERT_5_G Tentative Bond Valency for Co1       (II)      .       1.97 Info
PLAT883_ALERT_1_G No Info/Value for _atom_sites_solution_primary .     Please Do !
PLAT899_ALERT_4_G SHELXL2018 is Deprecated and Succeeded by SHELXL     2019/3 Note
PLAT909_ALERT_3_G Percentage of I>2sig(I) Data at Theta(Max) Still        50% Note
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          2 Note
                1  0  0,   0  0  2,
PLAT933_ALERT_2_G Number of HKL-OMIT Records in Embedded .res File          2 Note
                1  0  0,   0  0  2,
PLAT969_ALERT_5_G The 'Henn et al.' R-Factor-gap value ...........      3.953 Note
              Predicted wR2: Based on SigI   2  2.70 or SHELX Weight  9.36       
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          3 Info

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   4 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   9 ALERT level G = General information/check it is not something unexpected

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   3 ALERT type 2 Indicator that the structure model may be wrong or deficient
   5 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check


checkCIF publication errors

Alert level A
PUBL005_ALERT_1_A  _publ_contact_author_email, _publ_contact_author_fax and
            _publ_contact_author_phone are all missing.
            At least one of these should be present.

   1 ALERT level A = Data missing that is essential or data in wrong format
   0 ALERT level G = General alerts. Data that may be required is missing
# start Validation Reply Form
_vrf_PUBL005_GLOBAL
;
PROBLEM: _publ_contact_author_email, _publ_contact_author_fax and
RESPONSE: ...
;
# end Validation Reply Form 

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Reference check results

The following reference was not checked in detail as it was not recognized as a reference to a journal article

Sheldrick, G. M. (2018). SHELXL2018 Program for Crystal Structure Solution. University of G\"ottingen. [software reference?]

The following references do not appear to be cited

Lin, C.-Y., Fettinger, J. C. & Power, P. P. (2017). Inorg. Chem. 56, 9892--9902.

Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.

Sheldrick, G. M. (2015). Acta Cryst. C71, 3--8.

Citation comments

1 date found in data_I _publ_manuscript_text that could be part of a citation but not found in reference list: 2017

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Computing details

Triacetonitrile(1,4,7-trimethyl-1,4,7-triazacyclononane)cobalt(II) bis(tetraphenylborate)

Crystal data

[Co(C2H3N)3(C9H21N3)](C24H20B)2	F(000) = 2108
Mr = 991.80	Dx = 1.195 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
a = 18.1245 (16) Å	Cell parameters from 9821 reflections
b = 11.6689 (10) Å	θ = 2.2–24.7°
c = 26.067 (2) Å	µ = 0.36 mm^−1
β = 90.332 (2)°	T = 133 K
V = 5513.0 (8) Å^3	Platy, orange
Z = 4	0.10 × 0.09 × 0.05 mm

Data collection

Bruker APEXII CCD detector diffractometer	6984 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.096
phi and ω scans	θmax = 24.8°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −21→21
Tmin = 0.627, Tmax = 0.745	k = −13→13
112545 measured reflections	l = −30→30
9437 independent reflections

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.056	H-atom parameters constrained
wR(F^2) = 0.107	w = 1/[σ^2(Fo^2) + (0.033P)^2 + 3.7116P] where P = (Fo^2 + 2Fc^2)/3
S = 1.14	(Δ/σ)max < 0.001
9437 reflections	Δρmax = 0.59 e Å^−3
655 parameters	Δρmin = −0.63 e Å^−3

Special details

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. All H atoms were positioned with idealized geometry and refined isotropically with U_iso(H) = 1.2U_eq(C) using a riding model.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Co1	0.26079 (2)	0.21794 (3)	0.37198 (2)	0.02127 (11)
N1	0.36590 (12)	0.2774 (2)	0.34576 (9)	0.0289 (6)
N2	0.32689 (13)	0.1042 (2)	0.41730 (9)	0.0364 (6)
N3	0.27676 (13)	0.09052 (19)	0.31402 (8)	0.0297 (6)
N4	0.25061 (14)	0.3410 (2)	0.43183 (9)	0.0373 (6)
N5	0.20270 (13)	0.3280 (2)	0.32282 (9)	0.0324 (6)
N6	0.15961 (13)	0.1475 (2)	0.40119 (9)	0.0302 (6)
C1	0.37595 (19)	0.4025 (3)	0.34969 (14)	0.0500 (9)
H1A	0.422038	0.424526	0.332853	0.075*
H1B	0.378075	0.424796	0.385918	0.075*
H1C	0.334415	0.441435	0.332902	0.075*
C10	0.23835 (17)	0.4038 (3)	0.46362 (12)	0.0376 (8)
C2	0.42496 (16)	0.2172 (3)	0.37525 (12)	0.0445 (8)
H2A	0.465850	0.271200	0.382424	0.053*
H2B	0.444754	0.153452	0.354361	0.053*
C11	0.2220 (2)	0.4837 (3)	0.50480 (13)	0.0664 (12)
H11A	0.219402	0.561709	0.490959	0.100*
H11B	0.260938	0.479669	0.530955	0.100*
H11C	0.174521	0.463643	0.520243	0.100*
C12	0.17103 (16)	0.3839 (3)	0.29450 (11)	0.0292 (7)
C13	0.13107 (17)	0.4524 (3)	0.25734 (11)	0.0375 (8)
H13A	0.089775	0.490987	0.274242	0.056*
H13B	0.112109	0.402832	0.229941	0.056*
H13C	0.164259	0.509904	0.242679	0.056*
C14	0.11375 (16)	0.1172 (3)	0.42739 (11)	0.0292 (7)
C15	0.05684 (17)	0.0781 (3)	0.46240 (11)	0.0408 (8)
H15A	0.013637	0.128266	0.459471	0.061*
H15B	0.075843	0.080410	0.497662	0.061*
H15C	0.042689	−0.000565	0.453668	0.061*
C16	0.00729 (16)	0.8301 (3)	0.37025 (10)	0.0298 (7)
C17	−0.06356 (17)	0.8249 (3)	0.39156 (11)	0.0399 (8)
H17	−0.079004	0.755634	0.407378	0.048*
C18	−0.11219 (19)	0.9176 (3)	0.39040 (13)	0.0514 (10)
H18	−0.159485	0.910873	0.405629	0.062*
C19	−0.0918 (2)	1.0189 (3)	0.36720 (13)	0.0546 (11)
H19	−0.124900	1.081956	0.366144	0.066*
C20	−0.0233 (2)	1.0274 (3)	0.34574 (13)	0.0489 (9)
H20	−0.008721	1.096751	0.329605	0.059*
C21	0.02505 (17)	0.9348 (3)	0.34749 (11)	0.0369 (8)
H21	0.072390	0.943247	0.332497	0.044*
C22	0.02576 (14)	0.5992 (2)	0.36243 (10)	0.0242 (6)
C23	0.05553 (15)	0.4955 (2)	0.37991 (10)	0.0280 (7)
H23	0.096128	0.498067	0.403093	0.034*
C24	0.02860 (16)	0.3893 (3)	0.36499 (11)	0.0307 (7)
H24	0.050531	0.321261	0.378052	0.037*
C25	−0.02994 (16)	0.3825 (3)	0.33126 (11)	0.0343 (7)
H25	−0.048891	0.310153	0.320958	0.041*
C26	−0.06053 (16)	0.4821 (3)	0.31272 (12)	0.0357 (7)
H26	−0.100747	0.478443	0.289238	0.043*
C27	−0.03319 (15)	0.5880 (2)	0.32799 (11)	0.0304 (7)
H27	−0.055402	0.655411	0.314519	0.037*
C28	0.09238 (16)	0.7265 (3)	0.43650 (10)	0.0316 (7)
C29	0.14978 (18)	0.7970 (3)	0.45322 (11)	0.0398 (8)
H29	0.175407	0.841343	0.428474	0.048*
C30	0.1714 (2)	0.8056 (3)	0.50445 (12)	0.0496 (9)
H30	0.210939	0.854754	0.513967	0.060*
C31	0.1354 (2)	0.7431 (3)	0.54106 (12)	0.0546 (10)
H31	0.150092	0.747998	0.576031	0.065*
C32	0.0779 (2)	0.6732 (3)	0.52669 (12)	0.0555 (10)
H32	0.052427	0.629733	0.551826	0.067*
C33	0.05695 (18)	0.6660 (3)	0.47559 (11)	0.0441 (9)
H33	0.016674	0.617682	0.466679	0.053*
C34	0.13362 (14)	0.7270 (2)	0.33569 (10)	0.0247 (6)
C35	0.12318 (15)	0.7591 (2)	0.28431 (10)	0.0295 (7)
H35	0.075907	0.785862	0.273925	0.035*
C36	0.17851 (16)	0.7535 (2)	0.24803 (11)	0.0349 (8)
H36	0.168751	0.776946	0.213751	0.042*
C37	0.24763 (16)	0.7143 (3)	0.26137 (12)	0.0363 (8)
H37	0.285910	0.711189	0.236663	0.044*
C38	0.26038 (16)	0.6794 (2)	0.31121 (12)	0.0352 (8)
H38	0.307613	0.651257	0.320943	0.042*
C39	0.20450 (15)	0.6854 (2)	0.34707 (11)	0.0306 (7)
H39	0.214621	0.660199	0.381041	0.037*
C40	0.51258 (14)	0.7520 (2)	0.31920 (10)	0.0215 (6)
C41	0.49323 (14)	0.6505 (2)	0.29379 (10)	0.0256 (6)
H41	0.507706	0.579698	0.308791	0.031*
C42	0.45418 (14)	0.6477 (2)	0.24806 (10)	0.0261 (7)
H42	0.442318	0.576246	0.232589	0.031*
C43	0.43240 (14)	0.7490 (2)	0.22484 (10)	0.0249 (7)
H43	0.407080	0.748123	0.192831	0.030*
C44	0.44819 (14)	0.8509 (2)	0.24909 (10)	0.0254 (6)
H44	0.432404	0.921059	0.234134	0.031*
C45	0.48688 (14)	0.8523 (2)	0.29510 (10)	0.0254 (6)
H45	0.496444	0.923995	0.311034	0.030*
C46	0.49871 (15)	0.7112 (2)	0.41940 (10)	0.0246 (6)
C47	0.52292 (17)	0.6700 (2)	0.46687 (10)	0.0315 (7)
H47	0.574506	0.662922	0.472701	0.038*
C48	0.47564 (19)	0.6390 (3)	0.50568 (11)	0.0388 (8)
H48	0.494909	0.610553	0.537172	0.047*
C49	0.40053 (19)	0.6491 (3)	0.49892 (11)	0.0414 (8)
H49	0.367657	0.628399	0.525620	0.050*
C50	0.37390 (18)	0.6897 (3)	0.45288 (12)	0.0411 (8)
H50	0.322223	0.697581	0.447692	0.049*
C51	0.42219 (16)	0.7190 (2)	0.41404 (11)	0.0322 (7)
H51	0.402379	0.745589	0.382387	0.039*
C52	0.62601 (15)	0.6606 (2)	0.37250 (9)	0.0251 (6)
C53	0.70063 (16)	0.6897 (3)	0.36737 (11)	0.0357 (8)
H53	0.713522	0.768607	0.367493	0.043*
C54	0.75655 (18)	0.6100 (3)	0.36213 (12)	0.0446 (9)
H54	0.806155	0.635014	0.358631	0.054*
C55	0.74065 (19)	0.4944 (3)	0.36195 (11)	0.0447 (9)
H55	0.778641	0.439427	0.357178	0.054*
C56	0.66883 (18)	0.4603 (3)	0.36880 (10)	0.0374 (8)
H56	0.656977	0.381066	0.369708	0.045*
C57	0.61333 (16)	0.5420 (2)	0.37443 (10)	0.0297 (7)
H57	0.564322	0.516009	0.379859	0.036*
C58	0.58565 (15)	0.8834 (2)	0.38696 (10)	0.0248 (6)
C59	0.63458 (16)	0.9399 (3)	0.35433 (11)	0.0326 (7)
H59	0.650183	0.901700	0.324077	0.039*
C60	0.66161 (17)	1.0498 (3)	0.36415 (12)	0.0407 (8)
H60	0.696074	1.083950	0.341477	0.049*
C61	0.63802 (18)	1.1086 (3)	0.40693 (12)	0.0406 (8)
H61	0.656582	1.183091	0.414112	0.049*
C62	0.58764 (17)	1.0590 (3)	0.43899 (11)	0.0357 (8)
H62	0.569907	1.099913	0.467905	0.043*
C63	0.56245 (15)	0.9482 (2)	0.42911 (10)	0.0285 (7)
H63	0.527914	0.915169	0.452055	0.034*
B1	0.06470 (17)	0.7221 (3)	0.37633 (12)	0.0270 (7)
B2	0.55686 (17)	0.7525 (3)	0.37481 (12)	0.0241 (7)
C3	0.39592 (16)	0.1703 (3)	0.42524 (12)	0.0470 (9)
H3A	0.433697	0.120075	0.441105	0.056*
H3B	0.386375	0.234537	0.449104	0.056*
C4	0.29529 (19)	0.0746 (3)	0.46769 (12)	0.0538 (10)
H4A	0.331093	0.029267	0.487397	0.081*
H4B	0.250094	0.029752	0.462629	0.081*
H4C	0.283707	0.144979	0.486477	0.081*
C5	0.3405 (2)	−0.0026 (3)	0.38691 (13)	0.0509 (9)
H5A	0.337486	−0.069866	0.409939	0.061*
H5B	0.390920	0.000031	0.372569	0.061*
C6	0.2858 (2)	−0.0163 (3)	0.34395 (13)	0.0464 (9)
H6A	0.302433	−0.078417	0.320865	0.056*
H6B	0.237452	−0.039030	0.358283	0.056*
C7	0.21341 (17)	0.0771 (3)	0.27841 (12)	0.0462 (9)
H7A	0.220658	0.008683	0.257235	0.069*
H7B	0.209788	0.144769	0.256266	0.069*
H7C	0.167867	0.069012	0.298162	0.069*
C8	0.34430 (16)	0.1195 (2)	0.28411 (11)	0.0330 (7)
H8A	0.335250	0.103584	0.247305	0.040*
H8B	0.385719	0.070483	0.295726	0.040*
C9	0.36514 (16)	0.2438 (2)	0.29074 (11)	0.0325 (7)
H9A	0.414619	0.256903	0.275954	0.039*
H9B	0.329423	0.292381	0.271835	0.039*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Co1	0.0208 (2)	0.0226 (2)	0.02047 (19)	0.00069 (17)	0.00212 (14)	0.00164 (17)
N1	0.0234 (13)	0.0275 (13)	0.0360 (14)	−0.0043 (11)	0.0051 (10)	−0.0021 (12)
N2	0.0324 (15)	0.0413 (16)	0.0355 (15)	0.0051 (13)	−0.0033 (12)	0.0076 (12)
N3	0.0344 (14)	0.0260 (14)	0.0288 (13)	−0.0031 (11)	0.0036 (11)	−0.0040 (11)
N4	0.0403 (16)	0.0392 (16)	0.0326 (15)	−0.0025 (13)	0.0073 (12)	−0.0078 (13)
N5	0.0313 (15)	0.0370 (15)	0.0291 (14)	0.0077 (12)	0.0089 (12)	0.0084 (12)
N6	0.0264 (14)	0.0390 (15)	0.0253 (13)	−0.0038 (12)	0.0029 (11)	0.0062 (11)
C1	0.048 (2)	0.035 (2)	0.067 (2)	−0.0204 (17)	0.0163 (18)	−0.0089 (18)
C10	0.041 (2)	0.040 (2)	0.0316 (18)	−0.0055 (16)	0.0042 (15)	−0.0051 (16)
C2	0.0219 (17)	0.057 (2)	0.054 (2)	−0.0013 (17)	−0.0046 (15)	−0.0076 (18)
C11	0.090 (3)	0.062 (3)	0.047 (2)	−0.006 (2)	0.015 (2)	−0.029 (2)
C12	0.0309 (17)	0.0326 (18)	0.0243 (16)	0.0035 (14)	0.0084 (13)	0.0040 (14)
C13	0.046 (2)	0.0399 (19)	0.0263 (16)	0.0097 (16)	0.0008 (14)	0.0089 (14)
C14	0.0300 (17)	0.0325 (18)	0.0250 (16)	−0.0011 (14)	−0.0016 (14)	0.0003 (13)
C15	0.0392 (19)	0.052 (2)	0.0308 (17)	−0.0112 (16)	0.0117 (14)	0.0035 (15)
C16	0.0325 (18)	0.0333 (18)	0.0234 (15)	0.0018 (14)	−0.0018 (13)	−0.0101 (13)
C17	0.040 (2)	0.044 (2)	0.0358 (18)	0.0070 (16)	0.0046 (15)	−0.0113 (15)
C18	0.041 (2)	0.072 (3)	0.041 (2)	0.022 (2)	−0.0032 (16)	−0.027 (2)
C19	0.067 (3)	0.051 (3)	0.046 (2)	0.032 (2)	−0.021 (2)	−0.0253 (19)
C20	0.064 (3)	0.032 (2)	0.051 (2)	0.0128 (18)	−0.0193 (19)	−0.0105 (16)
C21	0.0397 (19)	0.0313 (18)	0.0395 (18)	0.0042 (15)	−0.0068 (15)	−0.0086 (15)
C22	0.0194 (15)	0.0308 (17)	0.0224 (15)	0.0029 (13)	0.0078 (12)	−0.0011 (12)
C23	0.0239 (16)	0.0351 (18)	0.0252 (16)	0.0017 (14)	0.0057 (12)	0.0031 (13)
C24	0.0321 (18)	0.0283 (17)	0.0319 (17)	0.0028 (14)	0.0092 (14)	0.0058 (13)
C25	0.0341 (18)	0.0279 (18)	0.0412 (19)	−0.0011 (15)	0.0068 (15)	−0.0024 (14)
C26	0.0284 (17)	0.0366 (19)	0.0419 (19)	0.0006 (15)	−0.0067 (14)	−0.0037 (15)
C27	0.0301 (17)	0.0269 (17)	0.0343 (17)	0.0037 (14)	0.0023 (14)	0.0014 (13)
C28	0.0349 (17)	0.0292 (17)	0.0308 (16)	0.0085 (15)	0.0023 (13)	−0.0058 (14)
C29	0.058 (2)	0.0297 (18)	0.0313 (17)	0.0019 (16)	−0.0079 (15)	0.0000 (14)
C30	0.075 (3)	0.034 (2)	0.040 (2)	0.0057 (18)	−0.0187 (18)	−0.0065 (16)
C31	0.095 (3)	0.046 (2)	0.0229 (18)	0.019 (2)	−0.0065 (19)	−0.0120 (16)
C32	0.076 (3)	0.063 (3)	0.0279 (19)	0.008 (2)	0.0200 (18)	−0.0055 (18)
C33	0.048 (2)	0.055 (2)	0.0297 (18)	0.0012 (17)	0.0155 (15)	−0.0088 (16)
C34	0.0256 (16)	0.0184 (15)	0.0300 (16)	−0.0022 (13)	−0.0003 (12)	−0.0018 (13)
C35	0.0261 (16)	0.0299 (17)	0.0323 (17)	0.0019 (13)	0.0021 (13)	−0.0006 (13)
C36	0.0357 (18)	0.0365 (19)	0.0325 (17)	−0.0021 (15)	0.0076 (14)	0.0009 (14)
C37	0.0286 (17)	0.0332 (18)	0.047 (2)	−0.0058 (15)	0.0144 (14)	−0.0107 (16)
C38	0.0247 (17)	0.0278 (17)	0.053 (2)	0.0010 (13)	0.0007 (15)	−0.0091 (15)
C39	0.0317 (18)	0.0242 (16)	0.0357 (17)	−0.0007 (13)	−0.0017 (14)	−0.0003 (13)
C40	0.0209 (14)	0.0212 (15)	0.0225 (14)	−0.0007 (12)	0.0078 (11)	0.0009 (11)
C41	0.0280 (16)	0.0218 (16)	0.0271 (16)	−0.0002 (13)	0.0044 (13)	0.0027 (12)
C42	0.0258 (16)	0.0269 (17)	0.0258 (16)	−0.0032 (13)	0.0039 (12)	−0.0047 (13)
C43	0.0217 (15)	0.0335 (18)	0.0195 (14)	0.0004 (13)	0.0029 (11)	−0.0011 (12)
C44	0.0262 (16)	0.0237 (16)	0.0264 (16)	0.0053 (13)	0.0036 (12)	0.0023 (13)
C45	0.0270 (16)	0.0233 (16)	0.0260 (16)	0.0018 (13)	0.0043 (13)	−0.0020 (12)
C46	0.0354 (17)	0.0149 (14)	0.0237 (15)	0.0004 (13)	0.0055 (12)	−0.0033 (12)
C47	0.0427 (19)	0.0285 (17)	0.0233 (16)	−0.0008 (14)	0.0029 (14)	−0.0019 (13)
C48	0.064 (2)	0.0301 (18)	0.0222 (16)	−0.0004 (17)	0.0052 (15)	0.0007 (13)
C49	0.061 (2)	0.0352 (19)	0.0285 (18)	−0.0084 (17)	0.0210 (16)	−0.0005 (14)
C50	0.0385 (19)	0.046 (2)	0.0393 (19)	−0.0042 (16)	0.0145 (15)	0.0001 (16)
C51	0.0381 (18)	0.0297 (17)	0.0290 (16)	0.0009 (15)	0.0058 (13)	0.0027 (14)
C52	0.0346 (17)	0.0275 (16)	0.0132 (13)	0.0027 (13)	0.0016 (12)	0.0004 (12)
C53	0.0365 (19)	0.0368 (19)	0.0337 (17)	0.0022 (15)	0.0021 (14)	0.0013 (14)
C54	0.0337 (19)	0.058 (2)	0.042 (2)	0.0105 (18)	0.0036 (15)	0.0015 (17)
C55	0.047 (2)	0.056 (2)	0.0312 (18)	0.0261 (19)	−0.0004 (16)	−0.0026 (16)
C56	0.058 (2)	0.0317 (18)	0.0225 (16)	0.0131 (17)	−0.0064 (15)	0.0002 (13)
C57	0.0377 (18)	0.0314 (18)	0.0199 (15)	0.0023 (15)	−0.0011 (13)	0.0019 (13)
C58	0.0280 (16)	0.0249 (16)	0.0215 (15)	0.0012 (13)	−0.0052 (12)	0.0041 (12)
C59	0.0366 (18)	0.0323 (18)	0.0287 (16)	−0.0026 (15)	−0.0041 (14)	0.0061 (14)
C60	0.041 (2)	0.037 (2)	0.044 (2)	−0.0097 (16)	−0.0089 (16)	0.0191 (16)
C61	0.052 (2)	0.0230 (17)	0.047 (2)	−0.0048 (16)	−0.0231 (17)	0.0055 (15)
C62	0.047 (2)	0.0253 (17)	0.0344 (18)	0.0056 (15)	−0.0154 (15)	−0.0024 (14)
C63	0.0336 (17)	0.0247 (16)	0.0273 (16)	0.0010 (14)	−0.0069 (13)	0.0038 (13)
B1	0.0265 (18)	0.0271 (18)	0.0274 (17)	0.0029 (16)	0.0015 (14)	−0.0014 (15)
B2	0.0295 (18)	0.0183 (17)	0.0244 (17)	−0.0005 (14)	0.0027 (14)	0.0007 (13)
C3	0.0270 (18)	0.072 (3)	0.042 (2)	0.0050 (17)	−0.0111 (15)	0.0013 (18)
C4	0.050 (2)	0.073 (3)	0.038 (2)	0.010 (2)	−0.0079 (16)	0.0277 (19)
C5	0.058 (2)	0.033 (2)	0.061 (2)	0.0158 (17)	0.0042 (19)	0.0135 (17)
C6	0.066 (2)	0.0246 (18)	0.048 (2)	−0.0005 (17)	0.0122 (18)	−0.0017 (15)
C7	0.046 (2)	0.059 (2)	0.0336 (18)	−0.0164 (18)	−0.0016 (16)	−0.0149 (17)
C8	0.0333 (17)	0.0351 (18)	0.0305 (17)	0.0034 (14)	0.0088 (13)	−0.0077 (14)
C9	0.0264 (16)	0.0389 (19)	0.0325 (17)	−0.0005 (14)	0.0150 (13)	0.0017 (14)

Geometric parameters (Å, º)

Co1—N1	2.143 (2)	C35—C36	1.384 (4)
Co1—N2	2.139 (2)	C35—H35	0.9500
Co1—N3	2.141 (2)	C36—C37	1.377 (4)
Co1—N4	2.129 (3)	C36—H36	0.9500
Co1—N5	2.094 (3)	C37—C38	1.380 (4)
Co1—N6	2.153 (2)	C37—H37	0.9500
N1—C1	1.475 (4)	C38—C39	1.384 (4)
N1—C9	1.487 (3)	C38—H38	0.9500
N1—C2	1.490 (4)	C39—H39	0.9500
N2—C4	1.477 (4)	C40—C41	1.401 (4)
N2—C3	1.483 (4)	C40—C45	1.406 (4)
N2—C5	1.498 (4)	C40—B2	1.653 (4)
N3—C6	1.479 (4)	C41—C42	1.383 (4)
N3—C7	1.480 (4)	C41—H41	0.9500
N3—C8	1.494 (3)	C42—C43	1.384 (4)
N4—C10	1.129 (4)	C42—H42	0.9500
N5—C12	1.138 (3)	C43—C44	1.376 (4)
N6—C14	1.135 (3)	C43—H43	0.9500
C1—H1A	0.9800	C44—C45	1.386 (4)
C1—H1B	0.9800	C44—H44	0.9500
C1—H1C	0.9800	C45—H45	0.9500
C10—C11	1.454 (4)	C46—C51	1.396 (4)
C2—C3	1.511 (4)	C46—C47	1.396 (4)
C2—H2A	0.9900	C46—B2	1.645 (4)
C2—H2B	0.9900	C47—C48	1.378 (4)
C11—H11A	0.9800	C47—H47	0.9500
C11—H11B	0.9800	C48—C49	1.377 (4)
C11—H11C	0.9800	C48—H48	0.9500
C12—C13	1.447 (4)	C49—C50	1.375 (4)
C13—H13A	0.9800	C49—H49	0.9500
C13—H13B	0.9800	C50—C51	1.385 (4)
C13—H13C	0.9800	C50—H50	0.9500
C14—C15	1.455 (4)	C51—H51	0.9500
C15—H15A	0.9800	C52—C53	1.402 (4)
C15—H15B	0.9800	C52—C57	1.404 (4)
C15—H15C	0.9800	C52—B2	1.651 (4)
C16—C21	1.397 (4)	C53—C54	1.383 (4)
C16—C17	1.403 (4)	C53—H53	0.9500
C16—B1	1.642 (4)	C54—C55	1.379 (5)
C17—C18	1.395 (4)	C54—H54	0.9500
C17—H17	0.9500	C55—C56	1.374 (4)
C18—C19	1.379 (5)	C55—H55	0.9500
C18—H18	0.9500	C56—C57	1.394 (4)
C19—C20	1.368 (5)	C56—H56	0.9500
C19—H19	0.9500	C57—H57	0.9500
C20—C21	1.392 (4)	C58—C59	1.398 (4)
C20—H20	0.9500	C58—C63	1.401 (4)
C21—H21	0.9500	C58—B2	1.644 (4)
C22—C27	1.398 (4)	C59—C60	1.396 (4)
C22—C23	1.399 (4)	C59—H59	0.9500
C22—B1	1.638 (4)	C60—C61	1.379 (4)
C23—C24	1.387 (4)	C60—H60	0.9500
C23—H23	0.9500	C61—C62	1.370 (4)
C24—C25	1.376 (4)	C61—H61	0.9500
C24—H24	0.9500	C62—C63	1.394 (4)
C25—C26	1.374 (4)	C62—H62	0.9500
C25—H25	0.9500	C63—H63	0.9500
C26—C27	1.389 (4)	C3—H3A	0.9900
C26—H26	0.9500	C3—H3B	0.9900
C27—H27	0.9500	C4—H4A	0.9800
C28—C29	1.394 (4)	C4—H4B	0.9800
C28—C33	1.399 (4)	C4—H4C	0.9800
C28—B1	1.645 (4)	C5—C6	1.500 (5)
C29—C30	1.393 (4)	C5—H5A	0.9900
C29—H29	0.9500	C5—H5B	0.9900
C30—C31	1.369 (5)	C6—H6A	0.9900
C30—H30	0.9500	C6—H6B	0.9900
C31—C32	1.374 (5)	C7—H7A	0.9800
C31—H31	0.9500	C7—H7B	0.9800
C32—C33	1.385 (4)	C7—H7C	0.9800
C32—H32	0.9500	C8—C9	1.508 (4)
C33—H33	0.9500	C8—H8A	0.9900
C34—C35	1.403 (4)	C8—H8B	0.9900
C34—C39	1.403 (4)	C9—H9A	0.9900
C34—B1	1.643 (4)	C9—H9B	0.9900
N5—Co1—N4	89.38 (10)	C38—C37—H37	120.6
N4—Co1—N2	93.69 (10)	C37—C38—C39	120.1 (3)
N5—Co1—N3	93.66 (9)	C37—C38—H38	119.9
N5—Co1—N1	92.93 (9)	C39—C38—H38	119.9
N4—Co1—N1	95.53 (9)	C38—C39—C34	123.2 (3)
N1—Co1—N2	83.16 (9)	C38—C39—H39	118.4
N1—Co1—N3	82.86 (9)	C34—C39—H39	118.4
N2—Co1—N3	83.18 (9)	C41—C40—C45	114.3 (2)
N1—Co1—N6	175.58 (9)	C41—C40—B2	122.4 (2)
N2—Co1—N5	175.23 (9)	C45—C40—B2	123.2 (2)
N3—Co1—N4	176.62 (10)	C42—C41—C40	123.6 (3)
N5—Co1—N6	91.39 (9)	C42—C41—H41	118.2
N4—Co1—N6	85.44 (9)	C40—C41—H41	118.2
N2—Co1—N6	92.49 (9)	C41—C42—C43	120.0 (3)
N3—Co1—N6	95.94 (9)	C41—C42—H42	120.0
C1—N1—C9	109.2 (2)	C43—C42—H42	120.0
C1—N1—C2	110.1 (2)	C44—C43—C42	118.6 (3)
C9—N1—C2	112.1 (2)	C44—C43—H43	120.7
C1—N1—Co1	114.07 (18)	C42—C43—H43	120.7
C9—N1—Co1	102.65 (16)	C43—C44—C45	120.7 (3)
C2—N1—Co1	108.68 (17)	C43—C44—H44	119.7
C4—N2—C3	109.2 (2)	C45—C44—H44	119.7
C4—N2—C5	110.0 (3)	C44—C45—C40	122.8 (3)
C3—N2—C5	111.4 (2)	C44—C45—H45	118.6
C4—N2—Co1	114.68 (19)	C40—C45—H45	118.6
C3—N2—Co1	102.92 (18)	C51—C46—C47	114.7 (2)
C5—N2—Co1	108.51 (18)	C51—C46—B2	123.4 (2)
C6—N3—C7	108.9 (2)	C47—C46—B2	121.8 (2)
C6—N3—C8	112.2 (2)	C48—C47—C46	123.2 (3)
C7—N3—C8	109.4 (2)	C48—C47—H47	118.4
C6—N3—Co1	103.20 (17)	C46—C47—H47	118.4
C7—N3—Co1	114.11 (18)	C49—C48—C47	120.1 (3)
C8—N3—Co1	109.00 (16)	C49—C48—H48	119.9
C10—N4—Co1	173.5 (3)	C47—C48—H48	119.9
C12—N5—Co1	176.8 (2)	C50—C49—C48	118.9 (3)
C14—N6—Co1	163.7 (2)	C50—C49—H49	120.6
N1—C1—H1A	109.5	C48—C49—H49	120.6
N1—C1—H1B	109.5	C49—C50—C51	120.2 (3)
H1A—C1—H1B	109.5	C49—C50—H50	119.9
N1—C1—H1C	109.5	C51—C50—H50	119.9
H1A—C1—H1C	109.5	C50—C51—C46	122.8 (3)
H1B—C1—H1C	109.5	C50—C51—H51	118.6
N4—C10—C11	179.4 (4)	C46—C51—H51	118.6
N1—C2—C3	111.3 (2)	C53—C52—C57	113.6 (3)
N1—C2—H2A	109.4	C53—C52—B2	125.4 (3)
C3—C2—H2A	109.4	C57—C52—B2	121.0 (2)
N1—C2—H2B	109.4	C54—C53—C52	123.7 (3)
C3—C2—H2B	109.4	C54—C53—H53	118.1
H2A—C2—H2B	108.0	C52—C53—H53	118.1
C10—C11—H11A	109.5	C55—C54—C53	120.3 (3)
C10—C11—H11B	109.5	C55—C54—H54	119.8
H11A—C11—H11B	109.5	C53—C54—H54	119.8
C10—C11—H11C	109.5	C56—C55—C54	118.7 (3)
H11A—C11—H11C	109.5	C56—C55—H55	120.6
H11B—C11—H11C	109.5	C54—C55—H55	120.6
N5—C12—C13	178.3 (3)	C55—C56—C57	120.0 (3)
C12—C13—H13A	109.5	C55—C56—H56	120.0
C12—C13—H13B	109.5	C57—C56—H56	120.0
H13A—C13—H13B	109.5	C56—C57—C52	123.5 (3)
C12—C13—H13C	109.5	C56—C57—H57	118.3
H13A—C13—H13C	109.5	C52—C57—H57	118.3
H13B—C13—H13C	109.5	C59—C58—C63	114.7 (3)
N6—C14—C15	178.0 (3)	C59—C58—B2	121.5 (2)
C14—C15—H15A	109.5	C63—C58—B2	123.8 (2)
C14—C15—H15B	109.5	C60—C59—C58	123.0 (3)
H15A—C15—H15B	109.5	C60—C59—H59	118.5
C14—C15—H15C	109.5	C58—C59—H59	118.5
H15A—C15—H15C	109.5	C61—C60—C59	119.7 (3)
H15B—C15—H15C	109.5	C61—C60—H60	120.2
C21—C16—C17	114.8 (3)	C59—C60—H60	120.2
C21—C16—B1	124.4 (3)	C62—C61—C60	119.6 (3)
C17—C16—B1	120.6 (3)	C62—C61—H61	120.2
C18—C17—C16	122.5 (3)	C60—C61—H61	120.2
C18—C17—H17	118.8	C61—C62—C63	119.9 (3)
C16—C17—H17	118.8	C61—C62—H62	120.1
C19—C18—C17	120.2 (3)	C63—C62—H62	120.1
C19—C18—H18	119.9	C62—C63—C58	123.1 (3)
C17—C18—H18	119.9	C62—C63—H63	118.5
C20—C19—C18	119.2 (3)	C58—C63—H63	118.5
C20—C19—H19	120.4	C22—B1—C16	112.3 (2)
C18—C19—H19	120.4	C22—B1—C34	102.5 (2)
C19—C20—C21	120.2 (3)	C16—B1—C34	113.3 (2)
C19—C20—H20	119.9	C22—B1—C28	111.5 (2)
C21—C20—H20	119.9	C16—B1—C28	104.9 (2)
C20—C21—C16	123.1 (3)	C34—B1—C28	112.6 (2)
C20—C21—H21	118.4	C58—B2—C46	109.9 (2)
C16—C21—H21	118.4	C58—B2—C52	111.7 (2)
C27—C22—C23	114.9 (3)	C46—B2—C52	109.0 (2)
C27—C22—B1	123.4 (3)	C58—B2—C40	108.9 (2)
C23—C22—B1	121.3 (2)	C46—B2—C40	108.0 (2)
C24—C23—C22	123.1 (3)	C52—B2—C40	109.3 (2)
C24—C23—H23	118.4	N2—C3—C2	111.5 (3)
C22—C23—H23	118.4	N2—C3—H3A	109.3
C25—C24—C23	119.9 (3)	C2—C3—H3A	109.3
C25—C24—H24	120.0	N2—C3—H3B	109.3
C23—C24—H24	120.0	C2—C3—H3B	109.3
C26—C25—C24	119.0 (3)	H3A—C3—H3B	108.0
C26—C25—H25	120.5	N2—C4—H4A	109.5
C24—C25—H25	120.5	N2—C4—H4B	109.5
C25—C26—C27	120.6 (3)	H4A—C4—H4B	109.5
C25—C26—H26	119.7	N2—C4—H4C	109.5
C27—C26—H26	119.7	H4A—C4—H4C	109.5
C26—C27—C22	122.5 (3)	H4B—C4—H4C	109.5
C26—C27—H27	118.7	N2—C5—C6	112.0 (3)
C22—C27—H27	118.7	N2—C5—H5A	109.2
C29—C28—C33	114.5 (3)	C6—C5—H5A	109.2
C29—C28—B1	122.6 (3)	N2—C5—H5B	109.2
C33—C28—B1	122.7 (3)	C6—C5—H5B	109.2
C30—C29—C28	123.2 (3)	H5A—C5—H5B	107.9
C30—C29—H29	118.4	N3—C6—C5	111.9 (3)
C28—C29—H29	118.4	N3—C6—H6A	109.2
C31—C30—C29	119.8 (3)	C5—C6—H6A	109.2
C31—C30—H30	120.1	N3—C6—H6B	109.2
C29—C30—H30	120.1	C5—C6—H6B	109.2
C30—C31—C32	119.3 (3)	H6A—C6—H6B	107.9
C30—C31—H31	120.3	N3—C7—H7A	109.5
C32—C31—H31	120.3	N3—C7—H7B	109.5
C31—C32—C33	120.1 (3)	H7A—C7—H7B	109.5
C31—C32—H32	120.0	N3—C7—H7C	109.5
C33—C32—H32	120.0	H7A—C7—H7C	109.5
C32—C33—C28	123.1 (3)	H7B—C7—H7C	109.5
C32—C33—H33	118.5	N3—C8—C9	111.3 (2)
C28—C33—H33	118.5	N3—C8—H8A	109.4
C35—C34—C39	114.4 (2)	C9—C8—H8A	109.4
C35—C34—B1	121.7 (2)	N3—C8—H8B	109.4
C39—C34—B1	123.4 (2)	C9—C8—H8B	109.4
C36—C35—C34	123.1 (3)	H8A—C8—H8B	108.0
C36—C35—H35	118.5	N1—C9—C8	111.4 (2)
C34—C35—H35	118.5	N1—C9—H9A	109.3
C37—C36—C35	120.3 (3)	C8—C9—H9A	109.3
C37—C36—H36	119.8	N1—C9—H9B	109.3
C35—C36—H36	119.8	C8—C9—H9B	109.3
C36—C37—C38	118.9 (3)	H9A—C9—H9B	108.0
C36—C37—H37	120.6
C1—N1—C2—C3	104.4 (3)	C27—C22—B1—C16	28.2 (3)
C9—N1—C2—C3	−133.9 (3)	C23—C22—B1—C16	−159.6 (2)
Co1—N1—C2—C3	−21.2 (3)	C27—C22—B1—C34	−93.6 (3)
C21—C16—C17—C18	−0.5 (4)	C23—C22—B1—C34	78.6 (3)
B1—C16—C17—C18	175.4 (3)	C27—C22—B1—C28	145.7 (2)
C16—C17—C18—C19	0.8 (5)	C23—C22—B1—C28	−42.2 (3)
C17—C18—C19—C20	−0.4 (5)	C21—C16—B1—C22	−137.0 (3)
C18—C19—C20—C21	−0.1 (5)	C17—C16—B1—C22	47.6 (3)
C19—C20—C21—C16	0.4 (5)	C21—C16—B1—C34	−21.5 (4)
C17—C16—C21—C20	−0.1 (4)	C17—C16—B1—C34	163.0 (3)
B1—C16—C21—C20	−175.8 (3)	C21—C16—B1—C28	101.7 (3)
C27—C22—C23—C24	−0.7 (4)	C17—C16—B1—C28	−73.7 (3)
B1—C22—C23—C24	−173.5 (2)	C35—C34—B1—C22	79.8 (3)
C22—C23—C24—C25	0.3 (4)	C39—C34—B1—C22	−91.3 (3)
C23—C24—C25—C26	0.3 (4)	C35—C34—B1—C16	−41.3 (4)
C24—C25—C26—C27	−0.4 (4)	C39—C34—B1—C16	147.6 (3)
C25—C26—C27—C22	−0.1 (4)	C35—C34—B1—C28	−160.2 (3)
C23—C22—C27—C26	0.6 (4)	C39—C34—B1—C28	28.7 (4)
B1—C22—C27—C26	173.2 (3)	C29—C28—B1—C22	154.6 (3)
C33—C28—C29—C30	1.1 (5)	C33—C28—B1—C22	−30.0 (4)
B1—C28—C29—C30	176.8 (3)	C29—C28—B1—C16	−83.6 (3)
C28—C29—C30—C31	−0.2 (5)	C33—C28—B1—C16	91.8 (3)
C29—C30—C31—C32	−0.5 (5)	C29—C28—B1—C34	40.0 (4)
C30—C31—C32—C33	0.3 (5)	C33—C28—B1—C34	−144.6 (3)
C31—C32—C33—C28	0.7 (5)	C59—C58—B2—C46	−178.8 (2)
C29—C28—C33—C32	−1.3 (5)	C63—C58—B2—C46	−0.6 (4)
B1—C28—C33—C32	−177.1 (3)	C59—C58—B2—C52	60.2 (3)
C39—C34—C35—C36	−1.8 (4)	C63—C58—B2—C52	−121.6 (3)
B1—C34—C35—C36	−173.6 (3)	C59—C58—B2—C40	−60.7 (3)
C34—C35—C36—C37	0.6 (4)	C63—C58—B2—C40	117.5 (3)
C35—C36—C37—C38	0.7 (4)	C51—C46—B2—C58	96.3 (3)
C36—C37—C38—C39	−0.7 (4)	C47—C46—B2—C58	−80.8 (3)
C37—C38—C39—C34	−0.6 (4)	C51—C46—B2—C52	−141.0 (3)
C35—C34—C39—C38	1.8 (4)	C47—C46—B2—C52	41.9 (3)
B1—C34—C39—C38	173.5 (3)	C51—C46—B2—C40	−22.4 (3)
C45—C40—C41—C42	1.9 (4)	C47—C46—B2—C40	160.5 (2)
B2—C40—C41—C42	177.9 (2)	C53—C52—B2—C58	−16.4 (4)
C40—C41—C42—C43	0.3 (4)	C57—C52—B2—C58	165.2 (2)
C41—C42—C43—C44	−2.2 (4)	C53—C52—B2—C46	−137.9 (3)
C42—C43—C44—C45	1.8 (4)	C57—C52—B2—C46	43.6 (3)
C43—C44—C45—C40	0.6 (4)	C53—C52—B2—C40	104.2 (3)
C41—C40—C45—C44	−2.4 (4)	C57—C52—B2—C40	−74.2 (3)
B2—C40—C45—C44	−178.4 (2)	C41—C40—B2—C58	168.1 (2)
C51—C46—C47—C48	0.1 (4)	C45—C40—B2—C58	−16.3 (3)
B2—C46—C47—C48	177.4 (3)	C41—C40—B2—C46	−72.7 (3)
C46—C47—C48—C49	−0.7 (5)	C45—C40—B2—C46	102.9 (3)
C47—C48—C49—C50	0.5 (5)	C41—C40—B2—C52	45.7 (3)
C48—C49—C50—C51	0.4 (5)	C45—C40—B2—C52	−138.6 (2)
C49—C50—C51—C46	−1.1 (5)	C4—N2—C3—C2	−172.0 (3)
C47—C46—C51—C50	0.8 (4)	C5—N2—C3—C2	66.3 (3)
B2—C46—C51—C50	−176.5 (3)	Co1—N2—C3—C2	−49.8 (3)
C57—C52—C53—C54	3.0 (4)	N1—C2—C3—N2	49.6 (4)
B2—C52—C53—C54	−175.5 (3)	C4—N2—C5—C6	106.9 (3)
C52—C53—C54—C55	−0.3 (5)	C3—N2—C5—C6	−131.9 (3)
C53—C54—C55—C56	−2.2 (5)	Co1—N2—C5—C6	−19.3 (3)
C54—C55—C56—C57	1.7 (4)	C7—N3—C6—C5	−170.4 (3)
C55—C56—C57—C52	1.3 (4)	C8—N3—C6—C5	68.4 (3)
C53—C52—C57—C56	−3.5 (4)	Co1—N3—C6—C5	−48.8 (3)
B2—C52—C57—C56	175.0 (2)	N2—C5—C6—N3	47.6 (4)
C63—C58—C59—C60	3.3 (4)	C6—N3—C8—C9	−132.8 (3)
B2—C58—C59—C60	−178.3 (3)	C7—N3—C8—C9	106.2 (3)
C58—C59—C60—C61	−2.1 (5)	Co1—N3—C8—C9	−19.1 (3)
C59—C60—C61—C62	−0.8 (5)	C1—N1—C9—C8	−171.9 (2)
C60—C61—C62—C63	2.1 (4)	C2—N1—C9—C8	65.9 (3)
C61—C62—C63—C58	−0.7 (4)	Co1—N1—C9—C8	−50.6 (2)
C59—C58—C63—C62	−2.0 (4)	N3—C8—C9—N1	48.6 (3)
B2—C58—C63—C62	179.7 (3)