Crystal structure of a dinuclear CoII complex with bridging fluoride ligands: di-μ-fluorido-bis­{tris­[(6-methyl­pyridin-2-yl)meth­yl]amine}­dicobalt(II) bis­(tetra­fluorido­borate)

Inomata, M.; Suenaga, Y.

doi:10.1107/S1600536814021631

metal-organic compounds

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ISSN: 2056-9890

Volume 70| Part 11| November 2014| Pages m359-m360

doi:10.1107/S1600536814021631

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Crystal structure of a dinuclear Co^II complex with bridging fluoride ligands: di-μ-fluorido-bis{tris[(6-methylpyridin-2-yl)methyl]amine}dicobalt(II) bis(tetrafluoridoborate)

Masataka Inomata ^a and Yusaku Suenaga ^a ^*

^aDepartment of Science, Kinki University, 3-4-1 Kowakae, Higashi-Osaka 577-8502, Japan
^*Correspondence e-mail: suenagay@chem.kindai.ac.jp

Edited by H. Ishida, Okayama University, Japan (Received 7 July 2014; accepted 1 October 2014; online 4 October 2014)

Reaction of Co(BF₄)₂·6H₂O with tris[(6-methylpyridin-2-yl)methyl]amiine in methanol results in a fluoride abstraction from BF₄⁻, yielding the unexpected title compound, [Co₂F₂(C₂₁H₂₄N₄)₂](BF₄)₂. The complex cation consists of two inversion-related [Co(C₂₁H₂₄N₄)]²⁺ moieties bridged by a pair of fluoride ligands. The Co^II cation is six-coordinated in a distorted octahedral geometry and forms a +II high-spin state. In the crystal, the complex cation and the BF₄⁻ anion are connected by C—H⋯F hydrogen bonds, forming a three-dimensional network. An intramolecular C—H⋯F hydrogen bond is also observed.

Keywords: crystal structure; dinuclear cobalt complex; fluoride bridge; high-spin Co^II complex; tripodal ligand; C—H⋯F hydrogen bonds.

CCDC reference: 1027138

1. Related literature

For related fluoride-bridging structures, see: Dugan et al. (2012 ); Ding et al. (2009 ). For related metal complexes with tripodal ligands, see: Massoud et al. (2008 ); Zhu et al. (2009 ); Beni et al. (2008 ).

2. Experimental

2.1. Crystal data

[Co₂F₂(C₂₁H₂₄N₄)₂](BF₄)₂
M_r = 994.36
Triclinic, $[P \overline 1]$
a = 8.7884 (17) Å
b = 11.334 (4) Å
c = 11.897 (2) Å
α = 64.91 (5)°
β = 82.04 (6)°
γ = 87.98 (7)°
V = 1062.5 (7) Å³
Z = 1
Mo Kα radiation
μ = 0.87 mm⁻¹
T = 120 K
0.20 × 0.20 × 0.10 mm

2.2. Data collection

Rigaku Mercury70 diffractometer
Absorption correction: multi-scan (REQAB; Rigaku, 1998 ) T_min = 0.787, T_max = 0.917
8221 measured reflections
4623 independent reflections
3660 reflections with F² > 2σ(F²)
R_int = 0.033

2.3. Refinement

R[F² > 2σ(F²)] = 0.053
wR(F²) = 0.157
S = 1.01
4623 reflections
289 parameters
H-atom parameters constrained
Δρ_max = 0.98 e Å⁻³
Δρ_min = −0.62 e Å⁻³

Table 1
Selected bond lengths (Å)

Co1—F1	1.985 (2)
Co1—F1ⁱ	2.098 (2)
Co1—N1	2.249 (3)
Co1—N2	2.143 (3)
Co1—N3	2.124 (3)
Co1—N4	2.251 (3)
Symmetry code: (i) -x, -y+1, -z.

Table 2
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C1—H1C⋯F1	0.98	2.37	3.298 (5)	157
C3—H3⋯F3ⁱⁱ	0.95	2.43	3.296 (5)	152
C5—H5⋯F5ⁱⁱⁱ	0.95	2.46	3.231 (6)	139
C10—H10⋯F2	0.95	2.52	3.372 (5)	149
C10—H10⋯F3	0.95	2.53	3.294 (5)	138
C12—H12⋯F2^iv	0.95	2.51	3.327 (5)	143
C14—H14A⋯F1	0.98	2.26	3.220 (4)	167
C14—H14C⋯F2^v	0.98	2.36	3.287 (4)	157
Symmetry codes: (ii) -x, -y+2, -z; (iii) -x+1, -y+2, -z; (iv) x-1, y, z; (v) -x, -y+1, -z+1.

Data collection: CrystalClear (Rigaku, 2008 ); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SIR2011 (Burla et al., 2012 ); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008 ); molecular graphics: CrystalStructure (Rigaku, 2014 ); software used to prepare material for publication: CrystalStructure.

Supporting information

CCDC reference: 1027138

Crystal structure: contains datablock I. DOI: 10.1107/S1600536814021631/is5368sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536814021631/is5368Isup2.hkl

Supporting information file. DOI: 10.1107/S1600536814021631/is5368Isup3.doc

checkCIF report

Related literature top

For related fluoride-bridging structures, see: Dugan et al. (2012); Ding et al. (2009). For related metal complexes with tripodal ligands, see: Massoud et al. (2008); Zhu et al. (2009); Beni et al. (2008).

Experimental top

A solution of Co(BF₄)₂·6H₂O (204 mg, 0.60 mmol) in dry methanol (20 ml) was added to a methanol solution (20 ml) of tris[(6-methylpyridin-2-yl)methyl]amiine (199 mg, 0.60 mmol). The resulting solution was stirred for 1 hr. Diethylether was added to the filtrate slowly to obtain the complex. This solution stand at ambient temperature and over the period of 7 days a purple microcrystals of [Co₂(Me₃tpa)₂F₂](BF₄)₂ separated from the solution in 18% (107 mg) yield. IR (KBr, cm^-1); 3448 s, 1605 s, 1578m, 1451 s, 1352m, 1084 s, 789m, 522m, ESI-MS; m/z=907.26(M—BF₄), Anal. Calc. for C₄₂H₄₈N₈F₂Co₂B₂F₈: C 50.73, H 4.87, N 11.27%. Found: C 50.96, H 4.63, N 11.07%.

Computing details top

Data collection: CrystalClear (Rigaku, 2008); cell refinement: CrystalClear (Rigaku, 2008); data reduction: CrystalClear (Rigaku, 2008); program(s) used to solve structure: SIR2011 (Burla et al., 2012); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2008); molecular graphics: CrystalStructure (Rigaku, 2014); software used to prepare material for publication: CrystalStructure (Rigaku, 2014).

Figures top

Perspective view of the complex showing 50% displacement ellipsoids. Hydrogen atoms are omitted for clarity.

Di-µ-fluorido-bis{tris[(6-methylpyridin-2-yl)methyl)amine}dicobalt(II) bis(tetrafluoridoborate) top

Crystal data top

[Co₂F₂(C₂₁H₂₄N₄)₂](BF₄)₂	Z = 1
M_r = 994.36	F(000) = 510.00
Triclinic, P1	D_x = 1.554 Mg m⁻³
a = 8.7884 (17) Å	Mo Kα radiation, λ = 0.71075 Å
b = 11.334 (4) Å	Cell parameters from 1627 reflections
c = 11.897 (2) Å	θ = 3.0–27.5°
α = 64.91 (5)°	µ = 0.87 mm⁻¹
β = 82.04 (6)°	T = 120 K
γ = 87.98 (7)°	Platelet, purple
V = 1062.5 (7) Å³	0.20 × 0.20 × 0.10 mm

Data collection top

Rigaku Mercury70 diffractometer	3660 reflections with F² > 2σ(F²)
Detector resolution: 7.314 pixels mm^-1	R_int = 0.033
ω scans	θ_max = 27.5°, θ_min = 3.0°
Absorption correction: multi-scan (REQAB; Rigaku, 1998)	h = −9→11
T_min = 0.787, T_max = 0.917	k = −14→14
8221 measured reflections	l = −12→15
4623 independent reflections

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.053	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.157	H-atom parameters constrained
S = 1.01	w = 1/[σ²(F_o²) + (0.1P)²] where P = (F_o² + 2F_c²)/3
4623 reflections	(Δ/σ)_max < 0.001
289 parameters	Δρ_max = 0.98 e Å⁻³
0 restraints	Δρ_min = −0.62 e Å⁻³
Primary atom site location: structure-invariant direct methods

Crystal data top

[Co₂F₂(C₂₁H₂₄N₄)₂](BF₄)₂	γ = 87.98 (7)°
M_r = 994.36	V = 1062.5 (7) Å³
Triclinic, P1	Z = 1
a = 8.7884 (17) Å	Mo Kα radiation
b = 11.334 (4) Å	µ = 0.87 mm⁻¹
c = 11.897 (2) Å	T = 120 K
α = 64.91 (5)°	0.20 × 0.20 × 0.10 mm
β = 82.04 (6)°

Data collection top

Rigaku Mercury70 diffractometer	4623 independent reflections
Absorption correction: multi-scan (REQAB; Rigaku, 1998)	3660 reflections with F² > 2σ(F²)
T_min = 0.787, T_max = 0.917	R_int = 0.033
8221 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.053	0 restraints
wR(F²) = 0.157	H-atom parameters constrained
S = 1.01	Δρ_max = 0.98 e Å⁻³
4623 reflections	Δρ_min = −0.62 e Å⁻³
289 parameters

Special details top

Refinement. Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F². R-factor (gt) are based on F. The threshold expression of F² > 2.0 σ(F²) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Co1	0.03362 (4)	0.54291 (4)	0.10441 (3)	0.01641 (16)
F1	−0.14216 (19)	0.48323 (17)	0.05164 (15)	0.0185 (4)
F2	0.4169 (3)	0.7066 (3)	0.4284 (2)	0.0545 (7)
F3	0.3216 (3)	0.8992 (3)	0.3089 (3)	0.0720 (10)
F4	0.5502 (3)	0.8964 (3)	0.3775 (2)	0.0501 (6)
F5	0.5324 (3)	0.8204 (3)	0.2337 (2)	0.0598 (8)
N1	0.1242 (3)	0.3500 (3)	0.2284 (2)	0.0201 (6)
N2	−0.0424 (3)	0.5803 (2)	0.2650 (2)	0.0163 (5)
N3	0.2518 (3)	0.5991 (3)	0.1259 (2)	0.0196 (5)
N4	0.0363 (3)	0.7600 (3)	−0.0106 (2)	0.0200 (5)
C1	−0.2383 (4)	0.7885 (4)	−0.0223 (3)	0.0269 (7)
C2	−0.0771 (4)	0.8417 (3)	−0.0566 (3)	0.0240 (7)
C3	−0.0463 (5)	0.9744 (3)	−0.1339 (3)	0.0323 (8)
C4	0.1020 (5)	1.0247 (4)	−0.1588 (3)	0.0355 (9)
C5	0.2178 (5)	0.9412 (4)	−0.1059 (3)	0.0328 (8)
C6	0.1820 (4)	0.8104 (3)	−0.0355 (3)	0.0236 (7)
C7	0.3070 (4)	0.7150 (3)	0.0098 (3)	0.0258 (7)
C8	0.2372 (3)	0.6245 (3)	0.2389 (3)	0.0217 (7)
C9	0.0739 (3)	0.6280 (3)	0.2991 (3)	0.0173 (6)
C10	0.0500 (4)	0.6739 (3)	0.3904 (3)	0.0218 (7)
C11	−0.0988 (4)	0.6703 (3)	0.4504 (3)	0.0237 (7)
C12	−0.2171 (4)	0.6211 (3)	0.4182 (3)	0.0243 (7)
C13	−0.1872 (4)	0.5767 (3)	0.3248 (3)	0.0192 (6)
C14	−0.3157 (4)	0.5238 (3)	0.2890 (3)	0.0246 (7)
C15	0.3529 (3)	0.4882 (3)	0.1383 (3)	0.0225 (7)
C16	0.2771 (4)	0.3608 (3)	0.2283 (3)	0.0228 (7)
C17	0.3622 (4)	0.2584 (4)	0.3017 (3)	0.0317 (8)
C18	0.2910 (5)	0.1365 (4)	0.3696 (4)	0.0367 (9)
C19	0.1369 (5)	0.1239 (4)	0.3671 (3)	0.0319 (8)
C20	0.0532 (4)	0.2333 (3)	0.2997 (3)	0.0247 (7)
C21	−0.1182 (4)	0.2238 (4)	0.3075 (3)	0.0296 (8)
B1	0.4541 (5)	0.8333 (4)	0.3389 (4)	0.0308 (9)
H1A	−0.29767	0.83787	−0.09082	0.0323*
H1B	−0.28508	0.79605	0.05397	0.0323*
H1C	−0.23792	0.69658	−0.00753	0.0323*
H3	−0.12718	1.02968	−0.1692	0.0388*
H4	0.12426	1.11443	−0.21091	0.0426*
H5	0.31982	0.97358	−0.11792	0.0394*
H7A	0.348	0.68666	−0.05641	0.0309*
H7B	0.39202	0.7586	0.02541	0.0309*
H8A	0.28931	0.70915	0.21639	0.0261*
H8B	0.2925	0.5563	0.30206	0.0261*
H10	0.13352	0.7073	0.41203	0.0261*
H11	−0.11794	0.7019	0.51321	0.0284*
H12	−0.31878	0.61724	0.45919	0.0292*
H14A	−0.27778	0.5055	0.21678	0.0295*
H14B	−0.39692	0.58799	0.26711	0.0295*
H14C	−0.35706	0.44322	0.35962	0.0295*
H15A	0.38062	0.48718	0.05522	0.0270*
H15B	0.44895	0.49994	0.16765	0.0270*
H17	0.46723	0.27156	0.30536	0.0381*
H18	0.34769	0.06351	0.41683	0.0440*
H19	0.08654	0.04083	0.411	0.0383*
H21A	−0.14588	0.24863	0.22358	0.0355*
H21B	−0.16664	0.28245	0.34239	0.0355*
H21C	−0.15395	0.13398	0.36185	0.0355*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0172 (3)	0.0196 (3)	0.0131 (2)	−0.00145 (16)	−0.00164 (15)	−0.00753 (17)
F1	0.0178 (9)	0.0233 (9)	0.0151 (8)	−0.0020 (7)	−0.0006 (7)	−0.0092 (7)
F2	0.0382 (13)	0.0528 (16)	0.0428 (14)	−0.0055 (12)	−0.0063 (11)	0.0091 (12)
F3	0.0525 (16)	0.0447 (16)	0.138 (3)	0.0222 (13)	−0.0531 (18)	−0.0473 (19)
F4	0.0437 (14)	0.0678 (18)	0.0561 (16)	−0.0020 (13)	−0.0153 (12)	−0.0399 (14)
F5	0.0763 (19)	0.0585 (17)	0.0446 (15)	−0.0296 (14)	0.0170 (13)	−0.0271 (13)
N1	0.0242 (14)	0.0230 (14)	0.0158 (12)	0.0022 (11)	−0.0044 (10)	−0.0106 (11)
N2	0.0175 (13)	0.0184 (13)	0.0122 (11)	0.0012 (10)	−0.0011 (9)	−0.0061 (10)
N3	0.0186 (13)	0.0256 (14)	0.0151 (12)	−0.0026 (11)	−0.0009 (10)	−0.0092 (11)
N4	0.0280 (14)	0.0176 (13)	0.0139 (12)	0.0008 (11)	−0.0009 (10)	−0.0068 (10)
C1	0.0287 (18)	0.0301 (19)	0.0240 (16)	0.0063 (14)	−0.0054 (14)	−0.0133 (14)
C2	0.0362 (19)	0.0224 (16)	0.0147 (14)	0.0004 (14)	−0.0031 (13)	−0.0093 (13)
C3	0.052 (2)	0.0202 (17)	0.0215 (16)	0.0070 (16)	−0.0100 (16)	−0.0050 (14)
C4	0.058 (3)	0.0219 (18)	0.0235 (17)	−0.0070 (17)	−0.0060 (17)	−0.0056 (14)
C5	0.044 (2)	0.0263 (18)	0.0262 (17)	−0.0134 (16)	0.0015 (15)	−0.0098 (15)
C6	0.0300 (18)	0.0227 (16)	0.0174 (15)	−0.0062 (14)	−0.0015 (13)	−0.0079 (13)
C7	0.0214 (17)	0.0293 (18)	0.0220 (16)	−0.0110 (14)	0.0033 (13)	−0.0074 (14)
C8	0.0177 (16)	0.0324 (18)	0.0216 (15)	−0.0040 (13)	−0.0036 (12)	−0.0171 (14)
C9	0.0209 (16)	0.0169 (14)	0.0128 (13)	0.0016 (12)	−0.0039 (11)	−0.0046 (11)
C10	0.0265 (17)	0.0226 (16)	0.0177 (15)	0.0002 (13)	−0.0062 (12)	−0.0090 (13)
C11	0.0320 (18)	0.0241 (17)	0.0186 (15)	0.0064 (14)	−0.0064 (13)	−0.0121 (13)
C12	0.0243 (17)	0.0288 (18)	0.0160 (15)	0.0042 (14)	−0.0017 (12)	−0.0064 (13)
C13	0.0214 (16)	0.0177 (15)	0.0156 (14)	0.0052 (12)	−0.0025 (12)	−0.0048 (12)
C14	0.0203 (16)	0.0320 (18)	0.0214 (16)	−0.0021 (14)	0.0014 (12)	−0.0122 (14)
C15	0.0153 (15)	0.0328 (18)	0.0263 (16)	0.0043 (13)	−0.0063 (12)	−0.0184 (14)
C16	0.0266 (17)	0.0280 (17)	0.0189 (15)	0.0066 (14)	−0.0072 (13)	−0.0142 (13)
C17	0.032 (2)	0.040 (2)	0.0297 (18)	0.0147 (17)	−0.0132 (15)	−0.0198 (17)
C18	0.049 (2)	0.036 (2)	0.0314 (19)	0.0254 (19)	−0.0175 (17)	−0.0188 (17)
C19	0.052 (2)	0.0240 (18)	0.0195 (16)	0.0086 (17)	−0.0076 (16)	−0.0090 (14)
C20	0.0370 (19)	0.0230 (17)	0.0130 (14)	0.0015 (14)	−0.0036 (13)	−0.0066 (13)
C21	0.039 (2)	0.0282 (18)	0.0187 (16)	−0.0073 (15)	0.0009 (14)	−0.0081 (14)
B1	0.027 (2)	0.034 (2)	0.035 (2)	0.0009 (17)	−0.0083 (17)	−0.0169 (18)

Geometric parameters (Å, º) top

Co1—F1	1.985 (2)	C8—H8B	0.990
Co1—F1ⁱ	2.098 (2)	C10—H10	0.950
Co1—N1	2.249 (3)	C11—H11	0.950
Co1—N2	2.143 (3)	C12—H12	0.950
Co1—N3	2.124 (3)	C14—H14A	0.980
Co1—N4	2.251 (3)	C14—H14B	0.980
C1—H1A	0.980	C14—H14C	0.980
C1—H1B	0.980	C15—H15A	0.990
C1—H1C	0.980	C15—H15B	0.990
C3—H3	0.950	C17—H17	0.950
C4—H4	0.950	C18—H18	0.950
C5—H5	0.950	C19—H19	0.950
C7—H7A	0.990	C21—H21A	0.980
C7—H7B	0.990	C21—H21B	0.980
C8—H8A	0.990	C21—H21C	0.980

C2—C1—H1A	109.475	C11—C12—H12	120.262
C2—C1—H1B	109.475	C13—C12—H12	120.262
C2—C1—H1C	109.470	C13—C14—H14A	109.477
H1A—C1—H1B	109.471	C13—C14—H14B	109.471
H1A—C1—H1C	109.471	C13—C14—H14C	109.474
H1B—C1—H1C	109.464	H14A—C14—H14B	109.469
C2—C3—H3	120.021	H14A—C14—H14C	109.471
C4—C3—H3	120.022	H14B—C14—H14C	109.466
C3—C4—H4	120.711	N3—C15—H15A	109.251
C5—C4—H4	120.709	N3—C15—H15B	109.254
C4—C5—H5	120.552	C16—C15—H15A	109.247
C6—C5—H5	120.552	C16—C15—H15B	109.257
N3—C7—H7A	109.158	H15A—C15—H15B	107.925
N3—C7—H7B	109.159	C16—C17—H17	120.594
C6—C7—H7A	109.163	C18—C17—H17	120.604
C6—C7—H7B	109.167	C17—C18—H18	120.738
H7A—C7—H7B	107.874	C19—C18—H18	120.746
N3—C8—H8A	108.359	C18—C19—H19	119.864
N3—C8—H8B	108.356	C20—C19—H19	119.859
C9—C8—H8A	108.352	C20—C21—H21A	109.472
C9—C8—H8B	108.358	C20—C21—H21B	109.469
H8A—C8—H8B	107.440	C20—C21—H21C	109.469
C9—C10—H10	120.591	H21A—C21—H21B	109.475
C11—C10—H10	120.590	H21A—C21—H21C	109.474
C10—C11—H11	120.224	H21B—C21—H21C	109.468
C12—C11—H11	120.224

F1—Co1—F1ⁱ—Co1ⁱ	0.00 (8)	C16—N1—C20—C21	175.4 (3)
F1ⁱ—Co1—F1—Co1ⁱ	0.00 (9)	C20—N1—C16—C15	174.2 (3)
F1—Co1—N1—C16	151.42 (17)	C20—N1—C16—C17	−2.5 (5)
F1—Co1—N1—C20	−29.6 (3)	Co1—N2—C9—C8	−10.8 (3)
N1—Co1—F1—Co1ⁱ	−86.50 (11)	Co1—N2—C9—C10	172.26 (16)
F1—Co1—N2—C9	−176.69 (11)	Co1—N2—C13—C12	−171.21 (15)
F1—Co1—N2—C13	−4.6 (2)	Co1—N2—C13—C14	8.8 (3)
N2—Co1—F1—Co1ⁱ	179.51 (7)	C9—N2—C13—C12	0.4 (3)
F1—Co1—N4—C2	28.6 (3)	C9—N2—C13—C14	−179.6 (2)
F1—Co1—N4—C6	−150.43 (17)	C13—N2—C9—C8	176.1 (2)
N4—Co1—F1—Co1ⁱ	87.98 (12)	C13—N2—C9—C10	−0.8 (4)
F1ⁱ—Co1—N1—C16	73.10 (19)	Co1—N3—C7—C6	42.6 (3)
F1ⁱ—Co1—N1—C20	−107.9 (3)	Co1—N3—C8—C9	−9.8 (3)
N1—Co1—F1ⁱ—Co1ⁱ	100.85 (12)	Co1—N3—C15—C16	−46.2 (3)
F1ⁱ—Co1—N3—C7	60.13 (17)	C7—N3—C8—C9	109.5 (3)
F1ⁱ—Co1—N3—C8	−177.16 (14)	C8—N3—C7—C6	−78.0 (3)
F1ⁱ—Co1—N3—C15	−57.08 (13)	C7—N3—C15—C16	−161.6 (3)
N3—Co1—F1ⁱ—Co1ⁱ	179.26 (9)	C15—N3—C7—C6	157.0 (3)
F1ⁱ—Co1—N4—C2	107.2 (3)	C8—N3—C15—C16	72.6 (3)
F1ⁱ—Co1—N4—C6	−71.84 (18)	C15—N3—C8—C9	−126.4 (2)
N4—Co1—F1ⁱ—Co1ⁱ	−102.42 (12)	Co1—N4—C2—C1	5.2 (5)
N1—Co1—N2—C9	82.20 (16)	Co1—N4—C2—C3	−175.7 (2)
N1—Co1—N2—C13	−105.7 (2)	Co1—N4—C6—C5	179.1 (2)
N2—Co1—N1—C16	−98.0 (2)	Co1—N4—C6—C7	3.4 (4)
N2—Co1—N1—C20	81.0 (3)	C2—N4—C6—C5	−0.1 (5)
N1—Co1—N3—C7	149.19 (19)	C2—N4—C6—C7	−175.8 (3)
N1—Co1—N3—C8	−88.09 (16)	C6—N4—C2—C1	−175.9 (3)
N1—Co1—N3—C15	31.99 (13)	C6—N4—C2—C3	3.3 (5)
N3—Co1—N1—C16	−14.90 (18)	N4—C2—C3—C4	−3.3 (6)
N3—Co1—N1—C20	164.1 (3)	C1—C2—C3—C4	175.8 (3)
N1—Co1—N4—C2	−165.2 (2)	C2—C3—C4—C5	0.1 (6)
N1—Co1—N4—C6	15.7 (4)	C3—C4—C5—C6	3.0 (6)
N4—Co1—N1—C16	−14.8 (4)	C4—C5—C6—N4	−3.1 (6)
N4—Co1—N1—C20	164.1 (2)	C4—C5—C6—C7	172.5 (3)
N2—Co1—N3—C7	−119.29 (18)	N4—C6—C7—N3	−31.1 (5)
N2—Co1—N3—C8	3.42 (14)	C5—C6—C7—N3	153.1 (3)
N2—Co1—N3—C15	123.50 (14)	N3—C8—C9—N2	14.5 (3)
N3—Co1—N2—C9	3.94 (14)	N3—C8—C9—C10	−168.5 (2)
N3—Co1—N2—C13	175.99 (19)	N2—C9—C10—C11	0.4 (4)
N2—Co1—N4—C2	−81.5 (3)	C8—C9—C10—C11	−176.5 (2)
N2—Co1—N4—C6	99.44 (19)	C9—C10—C11—C12	0.4 (4)
N4—Co1—N2—C9	−74.66 (17)	C10—C11—C12—C13	−0.8 (4)
N4—Co1—N2—C13	97.4 (2)	C11—C12—C13—N2	0.4 (4)
N3—Co1—N4—C2	−165.2 (3)	C11—C12—C13—C14	−179.6 (2)
N3—Co1—N4—C6	15.79 (17)	N3—C15—C16—N1	36.2 (5)
N4—Co1—N3—C7	−30.78 (17)	N3—C15—C16—C17	−147.1 (3)
N4—Co1—N3—C8	91.93 (17)	N1—C16—C17—C18	6.0 (6)
N4—Co1—N3—C15	−147.99 (15)	C15—C16—C17—C18	−170.5 (3)
Co1—N1—C16—C15	−6.7 (4)	C16—C17—C18—C19	−3.7 (6)
Co1—N1—C16—C17	176.6 (3)	C17—C18—C19—C20	−1.7 (6)
Co1—N1—C20—C19	177.9 (2)	C18—C19—C20—N1	5.4 (6)
Co1—N1—C20—C21	−3.5 (5)	C18—C19—C20—C21	−173.2 (4)
C16—N1—C20—C19	−3.2 (5)

Symmetry code: (i) −x, −y+1, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1C···F1	0.98	2.37	3.298 (5)	157
C3—H3···F3ⁱⁱ	0.95	2.43	3.296 (5)	152
C5—H5···F5ⁱⁱⁱ	0.95	2.46	3.231 (6)	139
C10—H10···F2	0.95	2.52	3.372 (5)	149
C10—H10···F3	0.95	2.53	3.294 (5)	138
C12—H12···F2^iv	0.95	2.51	3.327 (5)	143
C14—H14A···F1	0.98	2.26	3.220 (4)	167
C14—H14C···F2^v	0.98	2.36	3.287 (4)	157

Symmetry codes: (ii) −x, −y+2, −z; (iii) −x+1, −y+2, −z; (iv) x−1, y, z; (v) −x, −y+1, −z+1.

Selected bond lengths (Å) top

Co1—F1	1.985 (2)	Co1—N2	2.143 (3)
Co1—F1ⁱ	2.098 (2)	Co1—N3	2.124 (3)
Co1—N1	2.249 (3)	Co1—N4	2.251 (3)

Symmetry code: (i) −x, −y+1, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1C···F1	0.98	2.37	3.298 (5)	157
C3—H3···F3ⁱⁱ	0.95	2.43	3.296 (5)	152
C5—H5···F5ⁱⁱⁱ	0.95	2.456	3.231 (6)	139
C10—H10···F2	0.95	2.52	3.372 (5)	149
C10—H10···F3	0.95	2.53	3.294 (5)	138
C12—H12···F2^iv	0.95	2.51	3.327 (5)	143
C14—H14A···F1	0.98	2.26	3.220 (4)	167
C14—H14C···F2^v	0.98	2.36	3.287 (4)	157

Symmetry codes: (ii) −x, −y+2, −z; (iii) −x+1, −y+2, −z; (iv) x−1, y, z; (v) −x, −y+1, −z+1.

Acknowledgements

We gratefully acknowledge the School of Science and Engineering of Kinki University for funding this work.

References

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Volume 70| Part 11| November 2014| Pages m359-m360

doi:10.1107/S1600536814021631

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metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Crystal structure of a dinuclear CoII complex with bridging fluoride ligands: di-μ-fluorido-bis­­{tris­­[(6-methyl­pyridin-2-yl)meth­yl]amine}­dicobalt(II) bis­­(tetra­fluorido­borate)

1. Related literature

2. Experimental

2.1. Crystal data

2.2. Data collection

2.3. Refinement

Supporting information

Acknowledgements

References

metal-organic compounds

Crystal structure of a dinuclear Co^II complex with bridging fluoride ligands: di-μ-fluorido-bis{tris[(6-methylpyridin-2-yl)methyl]amine}dicobalt(II) bis(tetrafluoridoborate)