Acetonitrile-bis-(2,9-dimethyl-1,10-phen-an-throline)copper(II) bis-(tetra-fluorido-borate).

The title compound, [Cu(CH(3)CN)(C(12)H(12)N(2))(2)](BF(4))(2), crystallizes with two copper-containing cations and four tetra-fluoro-borate anions in the asymmetric unit. The structure represents a second crystal form of the salt, the first being an acetonitrile solvate [Watton (2009 ▶). Acta Cryst. E65, m585-m586]. The complex cation has a distorted trigonal-bipyramidal geometry, whereas the previous structure exhibits a distorted square-pyramidal geometry. One of the four BF(4) (-) counter-ions is disordered, with a refined site occupancy of 0.8615 (17):0.1385 (17).

Related literature

For the acetonitrile solvate structure, see: Watton (2009 ▶). For geometrical analysis, see: Addison et al. (1984 ▶); Holmes (1984 ▶); Watton (2010 ▶). For electrochemical behaviour of similar complexes, see: James & Williams (1961 ▶). For the characteristic colour of four-coordinate Cu(II) species, see: Miller et al. (1998 ▶).

Experimental

Crystal data

[Cu(C2H3N)(C12H12N2)2](BF4)2

M = 694.72

Monoclinic,

a = 14.7973 (3) Å

b = 18.5356 (3) Å

c = 22.5770 (4) Å

β = 105.2524 (18)°

V = 5974.23 (19) Å3

Z = 8

Mo Kα radiation

μ = 0.81 mm−1

T = 293 K

0.20 × 0.20 × 0.15 mm

Data collection

Oxford Diffraction Sapphire 3 diffractometer

Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006 ▶) T min = 0.765, T max = 1.000

40609 measured reflections

19629 independent reflections

13249 reflections with I > 2σ(I)

R int = 0.026

Refinement

R[F 2 > 2σ(F 2)] = 0.046

wR(F 2) = 0.122

S = 1.07

19629 reflections

855 parameters

30 restraints

H-atom parameters constrained

Δρmax = 1.06 e Å−3

Δρmin = −0.88 e Å−3

Data collection: CrysAlis CCD (Oxford Diffraction, 2006 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2006 ▶); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶).

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810042285/fj2351sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536810042285/fj2351Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Cu(C2H3N)(C12H12N2)2](BF4)2	F(000) = 2824
Mr = 694.72	Dx = 1.545 Mg m−3
Monoclinic, P21/c	Melting point: 573 K
Hall symbol: -P 2ybc	Mo Kα radiation, λ = 0.71073 Å
a = 14.7973 (3) Å	Cell parameters from 19467 reflections
b = 18.5356 (3) Å	θ = 4.3–32.6°
c = 22.5770 (4) Å	µ = 0.81 mm−1
β = 105.2524 (18)°	T = 293 K
V = 5974.23 (19) Å3	Block, green
Z = 8	0.20 × 0.20 × 0.15 mm

Oxford Diffraction Sapphire 3 diffractometer	19629 independent reflections
Radiation source: fine-focus sealed tube	13249 reflections with I > 2σ(I)
graphite	Rint = 0.026
ω scans	θmax = 32.7°, θmin = 4.3°
Absorption correction: multi-scan (CrysAlis RED; Oxford Diffraction, 2006)	h = −21→19
Tmin = 0.765, Tmax = 1.000	k = −22→28
40609 measured reflections	l = −31→34

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)] = 0.046	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.122	H-atom parameters constrained
S = 1.07	w = 1/[σ2(Fo2) + (0.0659P)2 + 0.084P] where P = (Fo2 + 2Fc2)/3
19629 reflections	(Δ/σ)max = 0.002
855 parameters	Δρmax = 1.06 e Å−3
30 restraints	Δρmin = −0.88 e Å−3

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

Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

	x	y	z	Uiso*/Ueq	Occ. (<1)
Cu1	0.084941 (15)	0.276621 (12)	0.343942 (10)	0.01537 (6)
N1	−0.00314 (10)	0.21950 (8)	0.27929 (7)	0.0154 (3)
N2	−0.03933 (11)	0.33834 (8)	0.33783 (7)	0.0162 (3)
N3	0.10759 (11)	0.20701 (8)	0.41990 (7)	0.0171 (3)
N4	0.18867 (11)	0.33074 (8)	0.40062 (7)	0.0169 (3)
N5	0.15524 (13)	0.29072 (10)	0.27572 (8)	0.0279 (4)
C1	0.01772 (13)	0.15984 (10)	0.25236 (8)	0.0183 (4)
C2	−0.04581 (14)	0.13204 (11)	0.19916 (9)	0.0219 (4)
H2	−0.0298	0.0913	0.1801	0.026*
C3	−0.13060 (14)	0.16454 (11)	0.17550 (9)	0.0217 (4)
H3	−0.1723	0.1458	0.1406	0.026*
C4	−0.15453 (13)	0.22663 (10)	0.20424 (8)	0.0182 (3)
C5	−0.24262 (14)	0.26302 (11)	0.18386 (9)	0.0229 (4)
H5	−0.2866	0.2465	0.1491	0.028*
C6	−0.26277 (14)	0.32106 (11)	0.21441 (9)	0.0235 (4)
H6	−0.3205	0.3438	0.2004	0.028*
C7	−0.19627 (13)	0.34786 (10)	0.26804 (8)	0.0187 (4)
C8	−0.21440 (14)	0.40614 (10)	0.30333 (9)	0.0215 (4)
H8	−0.2723	0.4291	0.2925	0.026*
C9	−0.14640 (14)	0.42887 (10)	0.35361 (9)	0.0214 (4)
H9	−0.1581	0.4676	0.3767	0.026*
C10	−0.05858 (13)	0.39375 (10)	0.37051 (8)	0.0180 (3)
C11	−0.10760 (12)	0.31515 (9)	0.28789 (8)	0.0154 (3)
C12	−0.08763 (12)	0.25267 (10)	0.25616 (8)	0.0151 (3)
C13	0.10864 (14)	0.12258 (11)	0.27908 (9)	0.0222 (4)
H13A	0.1407	0.1458	0.3168	0.033*
H13B	0.1467	0.1249	0.2506	0.033*
H13C	0.0971	0.0730	0.2871	0.033*
C14	0.01427 (14)	0.41765 (11)	0.42699 (9)	0.0239 (4)
H14A	0.0429	0.3761	0.4497	0.036*
H14B	−0.0148	0.4464	0.4522	0.036*
H14C	0.0612	0.4457	0.4152	0.036*
C15	0.06095 (15)	0.14918 (11)	0.43189 (9)	0.0229 (4)
C16	0.09939 (18)	0.10427 (12)	0.48283 (10)	0.0308 (5)
H16	0.0668	0.0636	0.4896	0.037*
C17	0.18394 (18)	0.12024 (12)	0.52207 (9)	0.0320 (5)
H17	0.2095	0.0900	0.5551	0.038*
C18	0.23232 (15)	0.18202 (11)	0.51279 (9)	0.0248 (4)
C19	0.31869 (16)	0.20535 (13)	0.55351 (9)	0.0303 (5)
H19	0.3467	0.1775	0.5877	0.036*
C20	0.35999 (15)	0.26690 (13)	0.54312 (9)	0.0311 (5)
H20	0.4167	0.2804	0.5699	0.037*
C21	0.31817 (13)	0.31238 (11)	0.49134 (9)	0.0237 (4)
C22	0.35496 (14)	0.37909 (13)	0.48009 (10)	0.0293 (5)
H22	0.4111	0.3955	0.5057	0.035*
C23	0.30806 (15)	0.41974 (12)	0.43140 (11)	0.0290 (5)
H23	0.3319	0.4645	0.4246	0.035*
C24	0.22373 (14)	0.39501 (11)	0.39107 (9)	0.0228 (4)
C25	0.23381 (13)	0.29031 (10)	0.45008 (8)	0.0182 (4)
C26	0.19076 (13)	0.22427 (10)	0.46050 (8)	0.0184 (4)
C27	−0.03382 (16)	0.13256 (12)	0.39053 (10)	0.0299 (5)
H27A	−0.0669	0.1768	0.3776	0.045*
H27B	−0.0684	0.1037	0.4123	0.045*
H27C	−0.0268	0.1065	0.3552	0.045*
C28	0.17413 (17)	0.43980 (12)	0.33721 (11)	0.0323 (5)
H28A	0.2048	0.4347	0.3049	0.048*
H28B	0.1754	0.4895	0.3493	0.048*
H28C	0.1103	0.4239	0.3229	0.048*
C29	0.17157 (15)	0.30088 (12)	0.22990 (10)	0.0259 (4)
C30	0.19169 (18)	0.31546 (13)	0.17158 (10)	0.0340 (5)
H30A	0.1536	0.3549	0.1516	0.051*
H30B	0.1781	0.2733	0.1460	0.051*
H30C	0.2566	0.3278	0.1785	0.051*
Cu2	0.389985 (16)	0.691709 (13)	0.105797 (10)	0.01934 (6)
N6	0.40860 (12)	0.80441 (10)	0.10026 (7)	0.0220 (3)
N7	0.27073 (11)	0.71383 (9)	0.04267 (7)	0.0196 (3)
N8	0.47331 (11)	0.63926 (9)	0.05485 (7)	0.0179 (3)
N9	0.49699 (12)	0.66233 (9)	0.17556 (7)	0.0220 (3)
N10	0.30781 (12)	0.63636 (10)	0.15327 (9)	0.0301 (4)
C31	0.47989 (15)	0.84849 (12)	0.12578 (9)	0.0258 (4)
C32	0.46991 (17)	0.92389 (13)	0.12152 (10)	0.0329 (5)
H32	0.5195	0.9534	0.1414	0.040*
C33	0.38771 (17)	0.95422 (12)	0.08832 (10)	0.0312 (5)
H33	0.3813	1.0041	0.0858	0.037*
C34	0.31299 (16)	0.90937 (11)	0.05798 (9)	0.0250 (4)
C35	0.22656 (17)	0.93593 (12)	0.01946 (10)	0.0291 (5)
H35	0.2177	0.9854	0.0141	0.035*
C36	0.15750 (16)	0.89042 (12)	−0.00933 (9)	0.0281 (4)
H36	0.1019	0.9090	−0.0340	0.034*
C37	0.16900 (14)	0.81373 (11)	−0.00228 (9)	0.0237 (4)
C38	0.10079 (15)	0.76359 (13)	−0.03216 (10)	0.0291 (5)
H38	0.0435	0.7795	−0.0567	0.035*
C39	0.11933 (15)	0.69138 (12)	−0.02494 (10)	0.0281 (4)
H39	0.0747	0.6581	−0.0450	0.034*
C40	0.20568 (14)	0.66717 (11)	0.01275 (9)	0.0231 (4)
C41	0.25367 (14)	0.78642 (10)	0.03519 (9)	0.0201 (4)
C42	0.32663 (14)	0.83454 (11)	0.06588 (9)	0.0209 (4)
C43	0.57260 (16)	0.81640 (14)	0.15865 (11)	0.0346 (5)
H43A	0.5715	0.8030	0.1995	0.052*
H43B	0.6213	0.8512	0.1606	0.052*
H43C	0.5844	0.7744	0.1369	0.052*
C44	0.22558 (15)	0.58754 (11)	0.01864 (11)	0.0288 (5)
H44A	0.2917	0.5800	0.0348	0.043*
H44B	0.2050	0.5652	−0.0210	0.043*
H44C	0.1928	0.5666	0.0459	0.043*
C45	0.46565 (14)	0.63376 (11)	−0.00539 (9)	0.0214 (4)
C46	0.52727 (15)	0.59019 (11)	−0.02811 (9)	0.0244 (4)
H46	0.5192	0.5858	−0.0702	0.029*
C47	0.59841 (15)	0.55459 (11)	0.01151 (10)	0.0258 (4)
H47	0.6391	0.5261	−0.0035	0.031*
C48	0.61049 (13)	0.56075 (10)	0.07503 (10)	0.0217 (4)
C49	0.68461 (14)	0.52621 (11)	0.11996 (11)	0.0281 (5)
H49	0.7267	0.4967	0.1072	0.034*
C50	0.69392 (14)	0.53596 (11)	0.18022 (11)	0.0300 (5)
H50	0.7417	0.5121	0.2085	0.036*
C51	0.63208 (14)	0.58223 (11)	0.20202 (10)	0.0251 (4)
C52	0.64206 (16)	0.59802 (12)	0.26422 (10)	0.0325 (5)
H52	0.6896	0.5765	0.2943	0.039*
C53	0.58196 (18)	0.64482 (13)	0.28023 (10)	0.0344 (5)
H53	0.5893	0.6557	0.3214	0.041*
C54	0.50824 (16)	0.67732 (12)	0.23509 (9)	0.0279 (5)
C55	0.55759 (13)	0.61575 (10)	0.15911 (9)	0.0195 (4)
C56	0.54592 (13)	0.60427 (10)	0.09476 (9)	0.0179 (3)
C57	0.39157 (16)	0.67533 (13)	−0.05023 (9)	0.0297 (5)
H57A	0.3345	0.6479	−0.0606	0.045*
H57B	0.4116	0.6844	−0.0867	0.045*
H57C	0.3810	0.7204	−0.0322	0.045*
C58	0.44347 (19)	0.72961 (14)	0.25291 (11)	0.0375 (6)
H58A	0.4054	0.7525	0.2168	0.056*
H58B	0.4793	0.7655	0.2797	0.056*
H58C	0.4040	0.7045	0.2737	0.056*
C59	0.27828 (14)	0.59525 (12)	0.18046 (10)	0.0264 (4)
C60	0.24070 (17)	0.54244 (13)	0.21520 (11)	0.0338 (5)
H60A	0.1794	0.5279	0.1919	0.051*
H60B	0.2367	0.5634	0.2533	0.051*
H60C	0.2812	0.5011	0.2234	0.051*
B1	0.14194 (16)	0.37274 (12)	0.59292 (10)	0.0216 (4)
F1	0.12278 (9)	0.31320 (6)	0.55422 (6)	0.0299 (3)
F2	0.15876 (12)	0.35016 (8)	0.65311 (6)	0.0456 (4)
F3	0.06508 (11)	0.41852 (8)	0.58040 (8)	0.0512 (4)
F4	0.22077 (11)	0.40904 (8)	0.58686 (8)	0.0469 (4)
B2	0.39281 (17)	0.60964 (13)	0.40230 (11)	0.0255 (5)
F5	0.33071 (12)	0.57495 (9)	0.35454 (8)	0.0605 (5)
F6	0.44297 (10)	0.55965 (8)	0.44397 (8)	0.0523 (5)
F7	0.33939 (13)	0.65099 (9)	0.43110 (7)	0.0565 (5)
F8	0.44967 (13)	0.65558 (14)	0.38094 (8)	0.0811 (7)
B3	0.98516 (18)	0.44247 (14)	0.15311 (12)	0.0312 (5)
F9	1.02798 (10)	0.48400 (8)	0.20389 (6)	0.0405 (3)
F10	0.98237 (12)	0.37088 (8)	0.16878 (8)	0.0501 (4)
F11	0.89527 (11)	0.46847 (9)	0.12734 (8)	0.0576 (5)
F12	1.03623 (13)	0.44934 (8)	0.10927 (7)	0.0522 (4)
B4	0.4382 (2)	0.44043 (18)	0.18722 (13)	0.0285 (7)	0.8615 (17)
F13	0.52285 (13)	0.41538 (11)	0.17988 (8)	0.0520 (5)	0.8615 (17)
F14	0.45417 (14)	0.49308 (11)	0.23150 (9)	0.0548 (5)	0.8615 (17)
F15	0.39075 (18)	0.38431 (14)	0.20358 (14)	0.0916 (10)	0.8615 (17)
F16	0.38341 (16)	0.46846 (12)	0.13232 (8)	0.0597 (6)	0.8615 (17)
B4A	0.4575 (11)	0.4282 (10)	0.2016 (7)	0.0285 (7)	0.1385 (17)
F13A	0.5483 (7)	0.4392 (7)	0.2375 (5)	0.0520 (5)	0.1385 (17)
F14A	0.4001 (8)	0.4306 (7)	0.2415 (5)	0.0548 (5)	0.1385 (17)
F15A	0.4589 (11)	0.3639 (7)	0.1725 (7)	0.0916 (10)	0.1385 (17)
F16A	0.4292 (10)	0.4821 (8)	0.1576 (5)	0.0597 (6)	0.1385 (17)

	U11	U22	U33	U12	U13	U23
Cu1	0.01123 (10)	0.01830 (11)	0.01463 (10)	−0.00064 (8)	−0.00004 (7)	0.00094 (8)
N1	0.0135 (7)	0.0177 (7)	0.0147 (6)	0.0018 (6)	0.0031 (5)	0.0010 (6)
N2	0.0138 (7)	0.0181 (7)	0.0157 (7)	−0.0008 (6)	0.0020 (5)	0.0006 (6)
N3	0.0175 (7)	0.0187 (7)	0.0154 (7)	0.0014 (6)	0.0051 (6)	0.0006 (6)
N4	0.0131 (7)	0.0185 (7)	0.0180 (7)	−0.0015 (6)	0.0025 (6)	−0.0015 (6)
N5	0.0222 (9)	0.0385 (10)	0.0216 (8)	−0.0094 (7)	0.0032 (7)	−0.0013 (7)
C1	0.0174 (9)	0.0192 (9)	0.0190 (8)	−0.0002 (7)	0.0059 (7)	0.0015 (7)
C2	0.0228 (10)	0.0211 (9)	0.0216 (9)	0.0002 (8)	0.0055 (7)	−0.0038 (7)
C3	0.0211 (9)	0.0232 (9)	0.0185 (8)	−0.0040 (8)	0.0010 (7)	−0.0031 (7)
C4	0.0171 (8)	0.0190 (9)	0.0161 (8)	−0.0003 (7)	0.0000 (6)	−0.0002 (7)
C5	0.0179 (9)	0.0242 (10)	0.0209 (9)	−0.0012 (7)	−0.0052 (7)	0.0003 (7)
C6	0.0148 (9)	0.0249 (10)	0.0253 (9)	0.0033 (7)	−0.0043 (7)	0.0021 (8)
C7	0.0145 (8)	0.0187 (9)	0.0210 (8)	0.0019 (7)	0.0014 (7)	0.0032 (7)
C8	0.0171 (9)	0.0198 (9)	0.0261 (9)	0.0052 (7)	0.0032 (7)	0.0024 (8)
C9	0.0231 (9)	0.0183 (9)	0.0226 (9)	0.0044 (8)	0.0055 (7)	−0.0014 (7)
C10	0.0184 (9)	0.0172 (8)	0.0173 (8)	0.0003 (7)	0.0027 (7)	0.0010 (7)
C11	0.0133 (8)	0.0167 (8)	0.0148 (7)	−0.0001 (6)	0.0009 (6)	0.0017 (6)
C12	0.0135 (8)	0.0157 (8)	0.0149 (7)	0.0000 (6)	0.0015 (6)	0.0018 (6)
C13	0.0187 (9)	0.0243 (10)	0.0241 (9)	0.0067 (8)	0.0063 (7)	0.0003 (8)
C14	0.0226 (10)	0.0245 (10)	0.0220 (9)	0.0023 (8)	0.0010 (7)	−0.0059 (8)
C15	0.0299 (11)	0.0206 (9)	0.0220 (9)	−0.0009 (8)	0.0135 (8)	−0.0007 (7)
C16	0.0479 (14)	0.0213 (10)	0.0282 (10)	0.0020 (10)	0.0190 (10)	0.0039 (8)
C17	0.0522 (15)	0.0266 (11)	0.0191 (9)	0.0173 (10)	0.0125 (9)	0.0055 (8)
C18	0.0311 (11)	0.0277 (10)	0.0145 (8)	0.0160 (9)	0.0044 (7)	−0.0007 (7)
C19	0.0315 (11)	0.0378 (12)	0.0171 (9)	0.0219 (10)	−0.0016 (8)	−0.0026 (8)
C20	0.0185 (10)	0.0506 (14)	0.0188 (9)	0.0160 (9)	−0.0045 (7)	−0.0125 (9)
C21	0.0145 (9)	0.0343 (11)	0.0208 (9)	0.0048 (8)	0.0018 (7)	−0.0129 (8)
C22	0.0152 (9)	0.0424 (13)	0.0299 (10)	−0.0038 (9)	0.0049 (8)	−0.0180 (10)
C23	0.0230 (10)	0.0279 (11)	0.0398 (12)	−0.0114 (9)	0.0147 (9)	−0.0133 (9)
C24	0.0197 (9)	0.0236 (9)	0.0274 (10)	−0.0028 (8)	0.0102 (8)	−0.0038 (8)
C25	0.0144 (8)	0.0228 (9)	0.0167 (8)	0.0045 (7)	0.0027 (6)	−0.0066 (7)
C26	0.0181 (9)	0.0205 (9)	0.0155 (8)	0.0074 (7)	0.0025 (6)	−0.0022 (7)
C27	0.0331 (12)	0.0303 (11)	0.0296 (10)	−0.0131 (9)	0.0144 (9)	−0.0023 (9)
C28	0.0337 (12)	0.0231 (10)	0.0419 (13)	−0.0039 (9)	0.0132 (10)	0.0066 (9)
C29	0.0227 (10)	0.0299 (10)	0.0244 (9)	−0.0084 (8)	0.0052 (8)	−0.0034 (8)
C30	0.0423 (14)	0.0395 (13)	0.0254 (10)	−0.0071 (11)	0.0180 (10)	−0.0009 (9)
Cu2	0.01406 (11)	0.02553 (13)	0.01898 (11)	0.00282 (9)	0.00535 (8)	0.00247 (9)
N6	0.0189 (8)	0.0301 (9)	0.0178 (7)	−0.0011 (7)	0.0060 (6)	0.0043 (7)
N7	0.0153 (7)	0.0230 (8)	0.0218 (7)	0.0026 (6)	0.0075 (6)	−0.0013 (6)
N8	0.0126 (7)	0.0236 (8)	0.0174 (7)	0.0002 (6)	0.0038 (6)	0.0034 (6)
N9	0.0208 (8)	0.0271 (8)	0.0179 (7)	−0.0022 (7)	0.0046 (6)	0.0041 (7)
N10	0.0184 (8)	0.0386 (10)	0.0336 (10)	0.0034 (8)	0.0074 (7)	0.0125 (8)
C31	0.0241 (10)	0.0348 (11)	0.0190 (9)	−0.0086 (9)	0.0065 (8)	0.0044 (8)
C32	0.0379 (13)	0.0366 (12)	0.0248 (10)	−0.0145 (10)	0.0090 (9)	0.0012 (9)
C33	0.0428 (13)	0.0244 (10)	0.0286 (10)	−0.0071 (10)	0.0134 (10)	0.0024 (9)
C34	0.0315 (11)	0.0248 (10)	0.0213 (9)	0.0007 (8)	0.0119 (8)	0.0035 (8)
C35	0.0360 (12)	0.0264 (10)	0.0273 (10)	0.0088 (9)	0.0122 (9)	0.0078 (9)
C36	0.0277 (11)	0.0328 (11)	0.0243 (9)	0.0118 (9)	0.0077 (8)	0.0073 (9)
C37	0.0202 (9)	0.0310 (11)	0.0206 (9)	0.0074 (8)	0.0064 (7)	0.0032 (8)
C38	0.0173 (9)	0.0431 (13)	0.0251 (10)	0.0065 (9)	0.0024 (8)	0.0010 (9)
C39	0.0175 (9)	0.0361 (12)	0.0294 (10)	0.0003 (9)	0.0037 (8)	−0.0063 (9)
C40	0.0169 (9)	0.0265 (10)	0.0277 (10)	0.0010 (8)	0.0091 (7)	−0.0040 (8)
C41	0.0182 (9)	0.0231 (9)	0.0204 (8)	0.0037 (7)	0.0077 (7)	0.0013 (7)
C42	0.0207 (9)	0.0255 (9)	0.0177 (8)	0.0013 (8)	0.0072 (7)	0.0027 (7)
C43	0.0228 (11)	0.0468 (14)	0.0307 (11)	−0.0119 (10)	0.0008 (9)	0.0114 (10)
C44	0.0233 (10)	0.0240 (10)	0.0401 (12)	0.0014 (8)	0.0105 (9)	−0.0064 (9)
C45	0.0177 (9)	0.0257 (10)	0.0214 (9)	−0.0038 (7)	0.0064 (7)	0.0022 (8)
C46	0.0281 (11)	0.0238 (10)	0.0256 (9)	−0.0064 (8)	0.0149 (8)	−0.0022 (8)
C47	0.0244 (10)	0.0202 (9)	0.0389 (11)	−0.0034 (8)	0.0192 (9)	−0.0026 (9)
C48	0.0131 (8)	0.0173 (9)	0.0360 (11)	−0.0020 (7)	0.0090 (8)	0.0017 (8)
C49	0.0139 (9)	0.0216 (10)	0.0482 (13)	0.0013 (7)	0.0069 (9)	0.0050 (9)
C50	0.0128 (9)	0.0232 (10)	0.0478 (13)	−0.0012 (7)	−0.0029 (8)	0.0110 (9)
C51	0.0166 (9)	0.0235 (10)	0.0305 (10)	−0.0066 (8)	−0.0021 (8)	0.0083 (8)
C52	0.0300 (12)	0.0310 (11)	0.0270 (10)	−0.0095 (9)	−0.0093 (9)	0.0090 (9)
C53	0.0420 (14)	0.0385 (13)	0.0176 (9)	−0.0142 (11)	−0.0012 (9)	0.0019 (9)
C54	0.0333 (12)	0.0307 (11)	0.0203 (9)	−0.0087 (9)	0.0082 (8)	0.0011 (8)
C55	0.0133 (8)	0.0227 (9)	0.0208 (8)	−0.0042 (7)	0.0013 (7)	0.0039 (7)
C56	0.0115 (8)	0.0193 (8)	0.0228 (8)	−0.0024 (7)	0.0043 (7)	0.0023 (7)
C57	0.0268 (11)	0.0416 (13)	0.0195 (9)	0.0035 (9)	0.0042 (8)	0.0065 (9)
C58	0.0497 (15)	0.0414 (13)	0.0269 (11)	−0.0018 (12)	0.0201 (11)	−0.0033 (10)
C59	0.0161 (9)	0.0357 (11)	0.0272 (10)	0.0022 (8)	0.0051 (8)	0.0062 (9)
C60	0.0294 (12)	0.0408 (13)	0.0340 (11)	−0.0063 (10)	0.0132 (9)	0.0082 (10)
B1	0.0192 (10)	0.0226 (10)	0.0212 (10)	0.0004 (8)	0.0023 (8)	−0.0028 (8)
F1	0.0321 (7)	0.0260 (6)	0.0290 (6)	0.0022 (5)	0.0038 (5)	−0.0085 (5)
F2	0.0631 (10)	0.0495 (9)	0.0227 (6)	−0.0056 (8)	0.0088 (7)	0.0003 (6)
F3	0.0365 (8)	0.0397 (8)	0.0613 (10)	0.0185 (7)	−0.0156 (7)	−0.0226 (7)
F4	0.0479 (9)	0.0371 (8)	0.0653 (10)	−0.0168 (7)	0.0318 (8)	−0.0054 (7)
B2	0.0199 (11)	0.0285 (12)	0.0270 (11)	−0.0070 (9)	0.0044 (9)	−0.0062 (9)
F5	0.0423 (9)	0.0589 (10)	0.0617 (11)	−0.0101 (8)	−0.0191 (8)	−0.0202 (9)
F6	0.0285 (8)	0.0289 (7)	0.0799 (12)	0.0035 (6)	−0.0205 (8)	−0.0045 (7)
F7	0.0745 (12)	0.0604 (10)	0.0370 (8)	0.0303 (9)	0.0188 (8)	0.0061 (8)
F8	0.0508 (11)	0.1460 (19)	0.0461 (10)	−0.0541 (12)	0.0120 (8)	0.0185 (11)
B3	0.0258 (12)	0.0322 (13)	0.0323 (12)	0.0063 (10)	0.0019 (10)	−0.0033 (11)
F9	0.0326 (8)	0.0498 (8)	0.0341 (7)	−0.0024 (6)	0.0000 (6)	−0.0082 (6)
F10	0.0499 (10)	0.0353 (8)	0.0658 (11)	−0.0008 (7)	0.0165 (8)	0.0064 (8)
F11	0.0312 (8)	0.0655 (11)	0.0608 (10)	0.0144 (8)	−0.0152 (7)	−0.0131 (9)
F12	0.0736 (12)	0.0443 (9)	0.0484 (9)	0.0118 (8)	0.0331 (9)	0.0023 (7)
B4	0.0280 (16)	0.0347 (17)	0.0206 (15)	−0.0020 (13)	0.0024 (12)	−0.0024 (13)
F13	0.0415 (11)	0.0712 (13)	0.0447 (10)	0.0222 (10)	0.0139 (8)	0.0047 (9)
F14	0.0473 (11)	0.0650 (12)	0.0449 (10)	0.0035 (9)	−0.0004 (9)	−0.0260 (9)
F15	0.0612 (16)	0.0842 (17)	0.120 (2)	−0.0425 (14)	0.0068 (15)	0.0368 (17)
F16	0.0703 (15)	0.0779 (14)	0.0236 (9)	0.0466 (12)	−0.0008 (9)	−0.0059 (9)
B4A	0.0280 (16)	0.0347 (17)	0.0206 (15)	−0.0020 (13)	0.0024 (12)	−0.0024 (13)
F13A	0.0415 (11)	0.0712 (13)	0.0447 (10)	0.0222 (10)	0.0139 (8)	0.0047 (9)
F14A	0.0473 (11)	0.0650 (12)	0.0449 (10)	0.0035 (9)	−0.0004 (9)	−0.0260 (9)
F15A	0.0612 (16)	0.0842 (17)	0.120 (2)	−0.0425 (14)	0.0068 (15)	0.0368 (17)
F16A	0.0703 (15)	0.0779 (14)	0.0236 (9)	0.0466 (12)	−0.0008 (9)	−0.0059 (9)

Cu1—N1	1.9872 (15)	N8—C56	1.370 (2)
Cu1—N4	1.9915 (15)	N9—C54	1.339 (3)
Cu1—N5	2.0895 (19)	N9—C55	1.365 (3)
Cu1—N3	2.1013 (15)	N10—C59	1.136 (3)
Cu1—N2	2.1391 (16)	C31—C32	1.406 (3)
N1—C1	1.337 (2)	C31—C43	1.500 (3)
N1—C12	1.368 (2)	C32—C33	1.370 (3)
N2—C10	1.338 (2)	C32—H32	0.9300
N2—C11	1.370 (2)	C33—C34	1.409 (3)
N3—C15	1.341 (3)	C33—H33	0.9300
N3—C26	1.365 (2)	C34—C42	1.406 (3)
N4—C24	1.339 (3)	C34—C35	1.431 (3)
N4—C25	1.365 (2)	C35—C36	1.352 (3)
N5—C29	1.138 (3)	C35—H35	0.9300
C1—C2	1.413 (3)	C36—C37	1.435 (3)
C1—C13	1.491 (3)	C36—H36	0.9300
C2—C3	1.367 (3)	C37—C38	1.407 (3)
C2—H2	0.9300	C37—C41	1.408 (3)
C3—C4	1.411 (3)	C38—C39	1.367 (3)
C3—H3	0.9300	C38—H38	0.9300
C4—C12	1.406 (2)	C39—C40	1.409 (3)
C4—C5	1.432 (3)	C39—H39	0.9300
C5—C6	1.353 (3)	C40—C44	1.504 (3)
C5—H5	0.9300	C41—C42	1.431 (3)
C6—C7	1.433 (3)	C43—H43A	0.9600
C6—H6	0.9300	C43—H43B	0.9600
C7—C11	1.407 (2)	C43—H43C	0.9600
C7—C8	1.409 (3)	C44—H44A	0.9600
C8—C9	1.370 (3)	C44—H44B	0.9600
C8—H8	0.9300	C44—H44C	0.9600
C9—C10	1.413 (3)	C45—C46	1.412 (3)
C9—H9	0.9300	C45—C57	1.495 (3)
C10—C14	1.504 (3)	C46—C47	1.359 (3)
C11—C12	1.433 (3)	C46—H46	0.9300
C13—H13A	0.9600	C47—C48	1.402 (3)
C13—H13B	0.9600	C47—H47	0.9300
C13—H13C	0.9600	C48—C56	1.409 (3)
C14—H14A	0.9600	C48—C49	1.434 (3)
C14—H14B	0.9600	C49—C50	1.343 (3)
C14—H14C	0.9600	C49—H49	0.9300
C15—C16	1.412 (3)	C50—C51	1.432 (3)
C15—C27	1.498 (3)	C50—H50	0.9300
C16—C17	1.362 (3)	C51—C52	1.404 (3)
C16—H16	0.9300	C51—C55	1.406 (3)
C17—C18	1.395 (3)	C52—C53	1.358 (4)
C17—H17	0.9300	C52—H52	0.9300
C18—C26	1.415 (3)	C53—C54	1.417 (3)
C18—C19	1.431 (3)	C53—H53	0.9300
C19—C20	1.344 (4)	C54—C58	1.491 (3)
C19—H19	0.9300	C55—C56	1.433 (3)
C20—C21	1.442 (3)	C57—H57A	0.9600
C20—H20	0.9300	C57—H57B	0.9600
C21—C22	1.401 (3)	C57—H57C	0.9600
C21—C25	1.408 (3)	C58—H58A	0.9600
C22—C23	1.363 (3)	C58—H58B	0.9600
C22—H22	0.9300	C58—H58C	0.9600
C23—C24	1.414 (3)	C59—C60	1.453 (3)
C23—H23	0.9300	C60—H60A	0.9600
C24—C28	1.495 (3)	C60—H60B	0.9600
C25—C26	1.428 (3)	C60—H60C	0.9600
C27—H27A	0.9600	B1—F2	1.381 (3)
C27—H27B	0.9600	B1—F4	1.384 (3)
C27—H27C	0.9600	B1—F3	1.387 (3)
C28—H28A	0.9600	B1—F1	1.390 (2)
C28—H28B	0.9600	B2—F8	1.371 (3)
C28—H28C	0.9600	B2—F5	1.378 (3)
C29—C30	1.450 (3)	B2—F7	1.380 (3)
C30—H30A	0.9600	B2—F6	1.388 (3)
C30—H30B	0.9600	B3—F10	1.377 (3)
C30—H30C	0.9600	B3—F9	1.388 (3)
Cu2—N9	1.9931 (16)	B3—F11	1.390 (3)
Cu2—N7	1.9976 (16)	B3—F12	1.400 (3)
Cu2—N10	2.0894 (19)	B4—F15	1.359 (4)
Cu2—N6	2.1150 (18)	B4—F14	1.372 (4)
Cu2—N8	2.1295 (16)	B4—F13	1.386 (4)
N6—C31	1.339 (3)	B4—F16	1.391 (3)
N6—C42	1.375 (2)	B4A—F15A	1.364 (15)
N7—C40	1.337 (3)	B4A—F13A	1.391 (14)
N7—C41	1.371 (2)	B4A—F16A	1.392 (14)
N8—C45	1.339 (2)	B4A—F14A	1.392 (15)
N1—Cu1—N4	170.39 (6)	C41—N7—Cu2	112.88 (13)
N1—Cu1—N5	83.26 (6)	C45—N8—C56	118.32 (17)
N4—Cu1—N5	87.80 (7)	C45—N8—Cu2	132.63 (13)
N1—Cu1—N3	101.85 (6)	C56—N8—Cu2	109.03 (12)
N4—Cu1—N3	81.63 (6)	C54—N9—C55	119.16 (18)
N5—Cu1—N3	132.45 (7)	C54—N9—Cu2	126.84 (15)
N1—Cu1—N2	81.43 (6)	C55—N9—Cu2	113.58 (12)
N4—Cu1—N2	106.03 (6)	C59—N10—Cu2	164.90 (18)
N5—Cu1—N2	118.15 (7)	N6—C31—C32	121.4 (2)
N3—Cu1—N2	109.32 (6)	N6—C31—C43	119.0 (2)
C1—N1—C12	119.70 (15)	C32—C31—C43	119.6 (2)
C1—N1—Cu1	126.13 (13)	C33—C32—C31	120.5 (2)
C12—N1—Cu1	113.46 (12)	C33—C32—H32	119.8
C10—N2—C11	118.46 (16)	C31—C32—H32	119.8
C10—N2—Cu1	132.76 (12)	C32—C33—C34	119.6 (2)
C11—N2—Cu1	108.70 (12)	C32—C33—H33	120.2
C15—N3—C26	118.22 (16)	C34—C33—H33	120.2
C15—N3—Cu1	132.51 (13)	C42—C34—C33	116.9 (2)
C26—N3—Cu1	109.04 (12)	C42—C34—C35	119.5 (2)
C24—N4—C25	119.56 (16)	C33—C34—C35	123.6 (2)
C24—N4—Cu1	127.61 (13)	C36—C35—C34	121.2 (2)
C25—N4—Cu1	112.19 (12)	C36—C35—H35	119.4
C29—N5—Cu1	163.05 (18)	C34—C35—H35	119.4
N1—C1—C2	120.44 (17)	C35—C36—C37	120.8 (2)
N1—C1—C13	119.39 (16)	C35—C36—H36	119.6
C2—C1—C13	120.17 (17)	C37—C36—H36	119.6
C3—C2—C1	120.55 (18)	C38—C37—C41	117.60 (19)
C3—C2—H2	119.7	C38—C37—C36	123.49 (19)
C1—C2—H2	119.7	C41—C37—C36	118.90 (19)
C2—C3—C4	119.67 (17)	C39—C38—C37	119.55 (19)
C2—C3—H3	120.2	C39—C38—H38	120.2
C4—C3—H3	120.2	C37—C38—H38	120.2
C12—C4—C3	117.16 (17)	C38—C39—C40	120.4 (2)
C12—C4—C5	119.21 (17)	C38—C39—H39	119.8
C3—C4—C5	123.62 (17)	C40—C39—H39	119.8
C6—C5—C4	120.99 (17)	N7—C40—C39	121.12 (19)
C6—C5—H5	119.5	N7—C40—C44	119.46 (18)
C4—C5—H5	119.5	C39—C40—C44	119.42 (19)
C5—C6—C7	120.79 (18)	N7—C41—C37	122.17 (18)
C5—C6—H6	119.6	N7—C41—C42	117.45 (17)
C7—C6—H6	119.6	C37—C41—C42	120.36 (18)
C11—C7—C8	116.77 (17)	N6—C42—C34	123.25 (19)
C11—C7—C6	119.68 (17)	N6—C42—C41	117.48 (18)
C8—C7—C6	123.55 (17)	C34—C42—C41	119.24 (18)
C9—C8—C7	119.77 (18)	C31—C43—H43A	109.5
C9—C8—H8	120.1	C31—C43—H43B	109.5
C7—C8—H8	120.1	H43A—C43—H43B	109.5
C8—C9—C10	120.32 (18)	C31—C43—H43C	109.5
C8—C9—H9	119.8	H43A—C43—H43C	109.5
C10—C9—H9	119.8	H43B—C43—H43C	109.5
N2—C10—C9	121.24 (17)	C40—C44—H44A	109.5
N2—C10—C14	118.98 (17)	C40—C44—H44B	109.5
C9—C10—C14	119.76 (17)	H44A—C44—H44B	109.5
N2—C11—C7	123.42 (17)	C40—C44—H44C	109.5
N2—C11—C12	117.43 (16)	H44A—C44—H44C	109.5
C7—C11—C12	119.11 (16)	H44B—C44—H44C	109.5
N1—C12—C4	122.45 (16)	N8—C45—C46	121.50 (18)
N1—C12—C11	117.41 (15)	N8—C45—C57	119.98 (18)
C4—C12—C11	120.12 (16)	C46—C45—C57	118.51 (18)
C1—C13—H13A	109.5	C47—C46—C45	120.06 (19)
C1—C13—H13B	109.5	C47—C46—H46	120.0
H13A—C13—H13B	109.5	C45—C46—H46	120.0
C1—C13—H13C	109.5	C46—C47—C48	120.11 (19)
H13A—C13—H13C	109.5	C46—C47—H47	119.9
H13B—C13—H13C	109.5	C48—C47—H47	119.9
C10—C14—H14A	109.5	C47—C48—C56	117.08 (18)
C10—C14—H14B	109.5	C47—C48—C49	123.72 (19)
H14A—C14—H14B	109.5	C56—C48—C49	119.20 (19)
C10—C14—H14C	109.5	C50—C49—C48	120.8 (2)
H14A—C14—H14C	109.5	C50—C49—H49	119.6
H14B—C14—H14C	109.5	C48—C49—H49	119.6
N3—C15—C16	121.1 (2)	C49—C50—C51	121.59 (19)
N3—C15—C27	119.07 (18)	C49—C50—H50	119.2
C16—C15—C27	119.79 (19)	C51—C50—H50	119.2
C17—C16—C15	120.4 (2)	C52—C51—C55	117.0 (2)
C17—C16—H16	119.8	C52—C51—C50	124.0 (2)
C15—C16—H16	119.8	C55—C51—C50	118.93 (19)
C16—C17—C18	120.03 (19)	C53—C52—C51	119.7 (2)
C16—C17—H17	120.0	C53—C52—H52	120.1
C18—C17—H17	120.0	C51—C52—H52	120.1
C17—C18—C26	116.87 (19)	C52—C53—C54	121.0 (2)
C17—C18—C19	123.94 (19)	C52—C53—H53	119.5
C26—C18—C19	119.2 (2)	C54—C53—H53	119.5
C20—C19—C18	120.98 (19)	N9—C54—C53	120.2 (2)
C20—C19—H19	119.5	N9—C54—C58	119.1 (2)
C18—C19—H19	119.5	C53—C54—C58	120.7 (2)
C19—C20—C21	121.33 (19)	N9—C55—C51	122.96 (18)
C19—C20—H20	119.3	N9—C55—C56	117.21 (16)
C21—C20—H20	119.3	C51—C55—C56	119.76 (18)
C22—C21—C25	117.11 (19)	N8—C56—C48	122.85 (17)
C22—C21—C20	123.96 (19)	N8—C56—C55	117.45 (17)
C25—C21—C20	118.9 (2)	C48—C56—C55	119.64 (17)
C23—C22—C21	119.65 (19)	C45—C57—H57A	109.5
C23—C22—H22	120.2	C45—C57—H57B	109.5
C21—C22—H22	120.2	H57A—C57—H57B	109.5
C22—C23—C24	121.1 (2)	C45—C57—H57C	109.5
C22—C23—H23	119.5	H57A—C57—H57C	109.5
C24—C23—H23	119.5	H57B—C57—H57C	109.5
N4—C24—C23	119.89 (19)	C54—C58—H58A	109.5
N4—C24—C28	119.77 (18)	C54—C58—H58B	109.5
C23—C24—C28	120.33 (19)	H58A—C58—H58B	109.5
N4—C25—C21	122.67 (18)	C54—C58—H58C	109.5
N4—C25—C26	117.53 (16)	H58A—C58—H58C	109.5
C21—C25—C26	119.77 (17)	H58B—C58—H58C	109.5
N3—C26—C18	123.20 (18)	N10—C59—C60	179.8 (3)
N3—C26—C25	116.92 (16)	C59—C60—H60A	109.5
C18—C26—C25	119.80 (18)	C59—C60—H60B	109.5
C15—C27—H27A	109.5	H60A—C60—H60B	109.5
C15—C27—H27B	109.5	C59—C60—H60C	109.5
H27A—C27—H27B	109.5	H60A—C60—H60C	109.5
C15—C27—H27C	109.5	H60B—C60—H60C	109.5
H27A—C27—H27C	109.5	F2—B1—F4	107.83 (18)
H27B—C27—H27C	109.5	F2—B1—F3	108.17 (19)
C24—C28—H28A	109.5	F4—B1—F3	110.45 (19)
C24—C28—H28B	109.5	F2—B1—F1	109.42 (18)
H28A—C28—H28B	109.5	F4—B1—F1	111.20 (18)
C24—C28—H28C	109.5	F3—B1—F1	109.69 (17)
H28A—C28—H28C	109.5	F8—B2—F5	111.0 (2)
H28B—C28—H28C	109.5	F8—B2—F7	107.5 (2)
N5—C29—C30	178.7 (3)	F5—B2—F7	106.3 (2)
C29—C30—H30A	109.5	F8—B2—F6	112.6 (2)
C29—C30—H30B	109.5	F5—B2—F6	110.27 (19)
H30A—C30—H30B	109.5	F7—B2—F6	108.77 (19)
C29—C30—H30C	109.5	F10—B3—F9	111.1 (2)
H30A—C30—H30C	109.5	F10—B3—F11	110.6 (2)
H30B—C30—H30C	109.5	F9—B3—F11	109.4 (2)
N9—Cu2—N7	171.49 (7)	F10—B3—F12	109.1 (2)
N9—Cu2—N10	84.78 (7)	F9—B3—F12	108.6 (2)
N7—Cu2—N10	86.72 (7)	F11—B3—F12	107.9 (2)
N9—Cu2—N6	103.17 (7)	F15—B4—F14	110.4 (3)
N7—Cu2—N6	81.92 (6)	F15—B4—F13	108.9 (3)
N10—Cu2—N6	128.15 (7)	F14—B4—F13	109.7 (2)
N9—Cu2—N8	81.35 (6)	F15—B4—F16	107.8 (3)
N7—Cu2—N8	103.69 (6)	F14—B4—F16	109.4 (3)
N10—Cu2—N8	123.42 (7)	F13—B4—F16	110.6 (2)
N6—Cu2—N8	108.43 (6)	F15A—B4A—F13A	105.9 (13)
C31—N6—C42	118.24 (18)	F15A—B4A—F16A	108.9 (13)
C31—N6—Cu2	132.65 (14)	F13A—B4A—F16A	112.0 (14)
C42—N6—Cu2	108.99 (13)	F15A—B4A—F14A	115.4 (15)
C40—N7—C41	119.19 (17)	F13A—B4A—F14A	106.1 (12)
C40—N7—Cu2	127.65 (14)	F16A—B4A—F14A	108.5 (13)