trans-Di­fluorido­tetra­kis­(pyridine-κN)chromium(III) perchlorate from synchrotron radiation

Moon, D.; Choi, J.-H.

doi:10.1107/S1600536813023052

metal-organic compounds

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ISSN: 2056-9890

Volume 69| Part 9| September 2013| Page m514

doi:10.1107/S1600536813023052

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trans-Difluoridotetrakis(pyridine-κN)chromium(III) perchlorate from synchrotron radiation

Dohyun Moon ^a and Jong-Ha Choi ^b ^*

^aPohang Accelerator Laboratory, POSTECH, Pohang 790-784, Republic of Korea, and ^bDepartment of Chemistry, Andong National University, Andong 760-749, Republic of Korea
^*Correspondence e-mail: jhchoi@andong.ac.kr

(Received 15 August 2013; accepted 16 August 2013; online 23 August 2013)

The are two independent complex cations in the title salt, [CrF₂(C₅H₅N)₄]ClO₄, each located on a centre of inversion, as well as an independent perchlorate counter-ion. The complex cations adopt slightly distorted octahedral coordination environments around the Cr^III ion, defined by four pyridine (py) N atoms in the equatorial plane and two F⁻ ligands in the axial positions; intramolecular C—H⋯F contacts are noted. The mean Cr—N(py) and Cr—F bond lengths are 2.088 (6) and 1.8559 (10) Å, respectively. The three-dimensional architecture is sustained by hydrogen bonds involving the pyridine C—H groups as donors, and F and O atoms as acceptors.

Related literature

For background to geometric isomerism in transition metal comlexes, see: Knight & Scott (2003 ); Ronconi & Sadler (2007 ). For the synthesis, see: Glerup et al. (1970 ). For the structure of trans-[Cr(py)₄F₂]PF₆, see: Fochi et al. (1991 ).

Experimental

Crystal data

[CrF₂(C₅H₅N)₄]ClO₄
M_r = 505.85
Triclinic, $[P \overline 1]$
a = 9.5690 (19) Å
b = 10.615 (2) Å
c = 12.663 (3) Å
α = 68.46 (3)°
β = 68.31 (3)°
γ = 79.38 (3)°
V = 1109.9 (5) Å³
Z = 2
Synchrotron radiation
λ = 0.63001 Å
μ = 0.49 mm⁻¹
T = 99 K
0.03 × 0.03 × 0.02 mm

Data collection

ADSC Q210 CCD area-detector
Absorption correction: empirical (HKL3000sm; Otwinowski & Minor, 1997 ) T_min = 0.985, T_max = 0.993
11523 measured reflections
5842 independent reflections
4912 reflections with I > 2σ(I)
R_int = 0.020

Refinement

R[F² > 2σ(F²)] = 0.036
wR(F²) = 0.099
S = 1.05
5842 reflections
293 parameters
H-atom parameters constrained
Δρ_max = 0.51 e Å⁻³
Δρ_min = −0.61 e Å⁻³

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C1—H1⋯F1	0.95	2.36	2.892 (2)	115
C6—H6⋯F1	0.95	2.31	2.874 (2)	118
C11—H11⋯F2	0.95	2.32	2.879 (2)	117
C16—H16⋯F2	0.95	2.39	2.915 (2)	115
C14—H14⋯O1P	0.95	2.61	3.154 (2)	117
C9—H9⋯O2P	0.95	2.63	3.320 (3)	130
C1—H1⋯O3Pⁱ	0.95	2.41	3.107 (2)	130
C4—H4⋯O1Pⁱⁱ	0.95	2.51	3.368 (2)	150
C5—H5⋯F1ⁱⁱⁱ	0.95	2.38	2.900 (2)	114
C10—H10⋯F1ⁱⁱⁱ	0.95	2.31	2.863 (2)	117
C15—H15⋯F2^iv	0.95	2.29	2.856 (2)	117
C20—H20⋯F2^iv	0.95	2.34	2.860 (2)	114
C15—H15⋯O3P^v	0.95	2.64	3.466 (2)	146
C19—H19⋯O2P^vi	0.95	2.58	3.227 (3)	125
Symmetry codes: (i) x-1, y+1, z; (ii) x-1, y, z; (iii) -x, -y+2, -z; (iv) -x, -y+2, -z+1; (v) -x+1, -y+1, -z+1; (vi) x, y+1, z.

Data collection: PAL ADSC Quantum-210 ADX Software (Arvai & Nielsen, 1983 ); cell refinement: HKL3000sm (Otwinowski & Minor, 1997); data reduction: HKL3000sm; program(s) used to solve structure: SHELX-2013-XS (Sheldrick, 2008 ); program(s) used to refine structure: SHELX-2013-XL (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2007 ); software used to prepare material for publication: WinGX (Farrugia, 2012 ).

Supporting information

Crystal structure: contains datablock I. DOI: 10.1107/S1600536813023052/tk5248sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536813023052/tk5248Isup2.hkl

checkCIF report

Comment top

The study of geometrical isomerism in octahedral transition metal complexes with mixed ligands has generated considerable interest, and has provided much basic structural information and spectroscopic properties (Knight & Scott, 2003). The geometry of various ligands in the metal complexes are very important in medical applications, and is likely to be a major factor in determining the anti-viral activity and its side-effects (Ronconi & Sadler, 2007). The [Cr(py)₄X₂]ⁿ⁺ cation (X = monodentate; py = pyridine) can be either trans or cis geometric isomers. The infrared, electronic absorption and emission spectroscopic properties are useful in distinguishing the geometric isomers of chromium(III) complexes. However, it should be noted that the geometric and conformational assignments based on spectroscopic properties are not always definitive.

In this communication, we describe the structure of trans-[Cr(py)₄F₂]ClO₄ in order to confirm the coordination of four pyridine molecules in equatorial plane and two fluoride ligands in axial positions. Counter anionic species play a very important role in coordination chemistry. This is another example of a trans-[Cr(py)₄F₂]⁺ structure but with a different counter anion.

The structural analysis shows the Cr^III complex cation to be coordinated by four nitrogen atoms of four py ligands in the equatorial sites and the two mutually trans fluoride atoms. The Cr1 and Cr2 complex cations are in half occupancy in the asymmetric unit. That is, each molecule is contributing a charge of +0.5. Thus, the salt comprises trans-[Cr(py)₄F₂]⁺ and ClO₄^-. An ellipsoid plot of one independent complex cation and the anion is depicted in Fig. 1.

Atoms Cr1 and Cr2 are located at a crystallographic center of symmetry, so these Cr complex cations have molecular C_i symmetry.

The Cr—N(py) distances vary from 2.0799 (17) to 2.0929 (15) Å and the Cr–F distances are in the range of 1.8552 (10) to 1.8566 (10) Å. These bond lengths are in good agreement with those observed in trans-[Cr(py)₄F₂]PF₆ (Fochi et al., 1991).

The ClO₄^- anion remains outside the coordination sphere. The crystal packing is stabilized by hydrogen bonding interactions between the C—H groups of the py ligand and the oxygens of the ClO₄^- anion, Table 1. As expected, the ClO₄^- counter ion has slightly distorted tetrahedral geometry due to the influence of hydrogen bonding on the Cl—O bond lengths and the O—Cl–O angles. Consideration of the crystal packing shows that intermolecular C—H···F hydrogen bonds are also present, Table 1.

Related literature top

For background to geometric isomerism in transition metal comlexes, see: Knight & Scott (2003); Ronconi & Sadler (2007). For the synthesis, see: Glerup et al. (1970). For the structure of trans-[Cr(py)₄F₂]PF₆, see: Fochi et al. (1991).

Experimental top

All chemicals were reagent grade materials and used without further purification. The trans-[Cr(py)₄F₂]ClO₄ salt was prepared as described previously (Glerup et al., 1970), and allowed to stand in 0.1 M HClO₄ solution at room temperature for 1-2 days to give very small crystals suitable for X-ray structural analysis.

Computing details top

Data collection: PAL ADSC Quantum-210 ADX Software (Arvai & Nielsen, 1983); cell refinement: HKL3000sm (Otwinowski & Minor, 1997); data reduction: HKL3000sm (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELX-2013-XS (Sheldrick, 2008); program(s) used to refine structure: SHELX-2013-XL (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2007); software used to prepare material for publication: WinGX (Farrugia, 2012).

Figures top

Fig. 1. A perspective drawing (50% probability level) of one independent complex cation and the unique perchlorate anion in the structure of trans-[Cr(py)₄F₂]ClO₄

trans-Difluoridotetrakis(pyridine-κN)chromium(III) perchlorate top

Crystal data top

[CrF₂(C₅H₅N)₄]ClO₄	Z = 2
M_r = 505.85	F(000) = 518
Triclinic, P1	D_x = 1.514 Mg m⁻³
Hall symbol: -P 1	Synchrotron radiation, λ = 0.63001 Å
a = 9.5690 (19) Å	Cell parameters from 33119 reflections
b = 10.615 (2) Å	θ = 0.4–33.6°
c = 12.663 (3) Å	µ = 0.49 mm⁻¹
α = 68.46 (3)°	T = 99 K
β = 68.31 (3)°	Pink, plate
γ = 79.38 (3)°	0.03 × 0.03 × 0.02 mm
V = 1109.9 (5) Å³

Data collection top

ADSC Q210 CCD area-detector diffractometer	4912 reflections with I > 2σ(I)
Radiation source: PLSII 2D bending magnet	R_int = 0.020
ω scan	θ_max = 26.0°, θ_min = 1.6°
Absorption correction: empirical (using intensity measurements) (HKL3000sm; Otwinowski & Minor, 1997)	h = −13→13
T_min = 0.985, T_max = 0.993	k = −14→14
11523 measured reflections	l = −17→17
5842 independent reflections

Refinement top

Refinement on F²	Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: full	H-atom parameters constrained
R[F² > 2σ(F²)] = 0.036	w = 1/[σ²(F_o²) + (0.0543P)² + 0.5188P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.099	(Δ/σ)_max = 0.001
S = 1.05	Δρ_max = 0.51 e Å⁻³
5842 reflections	Δρ_min = −0.61 e Å⁻³
293 parameters	Extinction correction: SHELXL, Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.062 (4)

Crystal data top

[CrF₂(C₅H₅N)₄]ClO₄	γ = 79.38 (3)°
M_r = 505.85	V = 1109.9 (5) Å³
Triclinic, P1	Z = 2
a = 9.5690 (19) Å	Synchrotron radiation, λ = 0.63001 Å
b = 10.615 (2) Å	µ = 0.49 mm⁻¹
c = 12.663 (3) Å	T = 99 K
α = 68.46 (3)°	0.03 × 0.03 × 0.02 mm
β = 68.31 (3)°

Data collection top

ADSC Q210 CCD area-detector diffractometer	5842 independent reflections
Absorption correction: empirical (using intensity measurements) (HKL3000sm; Otwinowski & Minor, 1997)	4912 reflections with I > 2σ(I)
T_min = 0.985, T_max = 0.993	R_int = 0.020
11523 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.036	0 restraints
wR(F²) = 0.099	H-atom parameters constrained
S = 1.05	Δρ_max = 0.51 e Å⁻³
5842 reflections	Δρ_min = −0.61 e Å⁻³
293 parameters

Special details top

Experimental. Since the Pohang Accelerator Laboratory goniostat has only one omega-axis, diffrn_measured_fraction_theta_full is not fully covered as 0.944, especially for the low symmetry such as a triclinic system. As this is an inherent problem, other command and option (such as OMIT) were not helpful to improve the completeness.

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.

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

	x	y	z	U_iso*/U_eq
Cr1	0.0000	1.0000	0.0000	0.01263 (9)
F1	0.01103 (10)	1.14193 (9)	0.04859 (8)	0.01655 (19)
N1	−0.16449 (15)	0.91455 (13)	0.16450 (12)	0.0144 (2)
C1	−0.24067 (17)	0.99130 (16)	0.23459 (14)	0.0160 (3)
H1	−0.2177	1.0836	0.2077	0.019*
C2	−0.35141 (18)	0.94021 (17)	0.34453 (15)	0.0184 (3)
H2	−0.4036	0.9969	0.3918	0.022*
C3	−0.38521 (19)	0.80573 (18)	0.38478 (15)	0.0206 (3)
H3	−0.4594	0.7682	0.4605	0.025*
C4	−0.30797 (19)	0.72648 (17)	0.31164 (16)	0.0213 (3)
H4	−0.3294	0.6341	0.3366	0.026*
C5	−0.19964 (18)	0.78444 (16)	0.20218 (15)	0.0177 (3)
H5	−0.1484	0.7307	0.1520	0.021*
N2	0.17550 (15)	0.89172 (13)	0.06286 (12)	0.0150 (3)
C6	0.24772 (18)	0.94873 (16)	0.10540 (14)	0.0182 (3)
H6	0.2131	1.0362	0.1120	0.022*
C7	0.37130 (19)	0.88404 (18)	0.14009 (16)	0.0212 (3)
H7	0.4210	0.9271	0.1691	0.025*
C8	0.42122 (19)	0.75607 (18)	0.13180 (15)	0.0214 (3)
H8	0.5052	0.7097	0.1556	0.026*
C9	0.34678 (19)	0.69668 (17)	0.08827 (16)	0.0210 (3)
H9	0.3789	0.6089	0.0817	0.025*
C10	0.22513 (18)	0.76705 (16)	0.05457 (15)	0.0181 (3)
H10	0.1746	0.7262	0.0245	0.022*
Cr2	0.0000	1.0000	0.5000	0.01280 (9)
F2	−0.15818 (10)	1.01373 (10)	0.44431 (8)	0.01706 (19)
N3	0.08874 (14)	0.82597 (13)	0.45187 (11)	0.0148 (3)
C11	0.02042 (18)	0.77691 (17)	0.40054 (15)	0.0179 (3)
H11	−0.0646	0.8267	0.3805	0.022*
C12	0.06960 (19)	0.65643 (17)	0.37590 (15)	0.0204 (3)
H12	0.0185	0.6242	0.3400	0.024*
C13	0.19391 (19)	0.58355 (17)	0.40415 (15)	0.0209 (3)
H13	0.2300	0.5010	0.3875	0.025*
C14	0.26469 (19)	0.63353 (17)	0.45721 (15)	0.0205 (3)
H14	0.3502	0.5855	0.4776	0.025*
C15	0.20934 (18)	0.75428 (17)	0.48022 (14)	0.0179 (3)
H15	0.2578	0.7877	0.5171	0.022*
N4	0.12228 (15)	1.12831 (14)	0.33344 (12)	0.0157 (3)
C16	0.05298 (18)	1.21171 (16)	0.25660 (14)	0.0177 (3)
H16	−0.0518	1.2052	0.2758	0.021*
C17	0.1294 (2)	1.30722 (17)	0.14993 (15)	0.0215 (3)
H17	0.0773	1.3660	0.0976	0.026*
C18	0.2822 (2)	1.31577 (18)	0.12077 (16)	0.0246 (4)
H18	0.3368	1.3805	0.0483	0.030*
C19	0.3546 (2)	1.2278 (2)	0.19953 (17)	0.0263 (4)
H19	0.4600	1.2304	0.1809	0.032*
C20	0.27139 (18)	1.13681 (18)	0.30494 (15)	0.0211 (3)
H20	0.3208	1.0781	0.3593	0.025*
Cl1P	0.64390 (4)	0.40483 (4)	0.24420 (3)	0.01718 (10)
O1P	0.53210 (15)	0.45637 (14)	0.33397 (13)	0.0305 (3)
O2P	0.5964 (2)	0.44001 (15)	0.14139 (13)	0.0374 (4)
O3P	0.66002 (17)	0.26002 (13)	0.29401 (13)	0.0304 (3)
O4P	0.78435 (15)	0.46338 (17)	0.20959 (16)	0.0387 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cr1	0.01311 (16)	0.01227 (16)	0.01356 (16)	0.00203 (12)	−0.00396 (13)	−0.00714 (12)
F1	0.0183 (4)	0.0153 (4)	0.0190 (4)	0.0016 (3)	−0.0062 (4)	−0.0100 (3)
N1	0.0146 (6)	0.0150 (6)	0.0150 (6)	0.0008 (5)	−0.0050 (5)	−0.0071 (5)
C1	0.0153 (7)	0.0167 (7)	0.0178 (7)	0.0020 (5)	−0.0060 (6)	−0.0086 (6)
C2	0.0142 (7)	0.0245 (8)	0.0184 (7)	0.0011 (6)	−0.0046 (6)	−0.0110 (6)
C3	0.0161 (7)	0.0263 (8)	0.0183 (7)	−0.0041 (6)	−0.0036 (6)	−0.0067 (6)
C4	0.0225 (8)	0.0195 (8)	0.0223 (8)	−0.0046 (6)	−0.0066 (7)	−0.0063 (6)
C5	0.0197 (7)	0.0157 (7)	0.0195 (7)	0.0000 (6)	−0.0065 (6)	−0.0081 (6)
N2	0.0149 (6)	0.0152 (6)	0.0149 (6)	0.0021 (5)	−0.0042 (5)	−0.0069 (5)
C6	0.0188 (7)	0.0180 (7)	0.0182 (7)	0.0018 (6)	−0.0054 (6)	−0.0085 (6)
C7	0.0196 (7)	0.0241 (8)	0.0227 (8)	0.0014 (6)	−0.0089 (7)	−0.0101 (6)
C8	0.0176 (7)	0.0234 (8)	0.0212 (8)	0.0047 (6)	−0.0068 (6)	−0.0075 (6)
C9	0.0198 (7)	0.0193 (7)	0.0230 (8)	0.0061 (6)	−0.0067 (7)	−0.0098 (6)
C10	0.0185 (7)	0.0170 (7)	0.0188 (7)	0.0022 (6)	−0.0053 (6)	−0.0083 (6)
Cr2	0.00999 (15)	0.01573 (17)	0.01295 (16)	0.00214 (12)	−0.00418 (12)	−0.00595 (12)
F2	0.0138 (4)	0.0204 (5)	0.0191 (4)	0.0021 (3)	−0.0077 (4)	−0.0080 (4)
N3	0.0133 (6)	0.0163 (6)	0.0135 (6)	0.0011 (5)	−0.0033 (5)	−0.0057 (5)
C11	0.0153 (7)	0.0199 (7)	0.0187 (7)	0.0013 (6)	−0.0056 (6)	−0.0076 (6)
C12	0.0190 (7)	0.0213 (8)	0.0225 (8)	0.0003 (6)	−0.0065 (6)	−0.0101 (6)
C13	0.0200 (7)	0.0180 (7)	0.0218 (8)	0.0023 (6)	−0.0035 (6)	−0.0084 (6)
C14	0.0172 (7)	0.0214 (8)	0.0198 (7)	0.0056 (6)	−0.0053 (6)	−0.0072 (6)
C15	0.0146 (7)	0.0220 (8)	0.0176 (7)	0.0033 (6)	−0.0055 (6)	−0.0087 (6)
N4	0.0140 (6)	0.0183 (6)	0.0149 (6)	0.0007 (5)	−0.0035 (5)	−0.0076 (5)
C16	0.0175 (7)	0.0193 (7)	0.0165 (7)	0.0023 (6)	−0.0056 (6)	−0.0077 (6)
C17	0.0266 (8)	0.0191 (7)	0.0178 (7)	0.0018 (6)	−0.0068 (7)	−0.0068 (6)
C18	0.0272 (9)	0.0224 (8)	0.0196 (8)	−0.0054 (7)	−0.0003 (7)	−0.0073 (6)
C19	0.0183 (8)	0.0327 (10)	0.0242 (8)	−0.0051 (7)	−0.0013 (7)	−0.0090 (7)
C20	0.0149 (7)	0.0275 (8)	0.0194 (7)	−0.0010 (6)	−0.0046 (6)	−0.0073 (6)
Cl1P	0.01680 (17)	0.01445 (17)	0.02051 (18)	0.00369 (12)	−0.00615 (14)	−0.00815 (13)
O1P	0.0234 (6)	0.0276 (7)	0.0369 (8)	0.0019 (5)	0.0019 (6)	−0.0201 (6)
O2P	0.0580 (10)	0.0308 (8)	0.0269 (7)	−0.0049 (7)	−0.0253 (7)	−0.0007 (6)
O3P	0.0427 (8)	0.0139 (6)	0.0382 (8)	0.0093 (5)	−0.0219 (7)	−0.0092 (5)
O4P	0.0178 (6)	0.0411 (8)	0.0597 (10)	−0.0049 (6)	−0.0017 (7)	−0.0291 (8)

Geometric parameters (Å, º) top

Cr1—F1ⁱ	1.8566 (10)	Cr2—N4	2.0799 (17)
Cr1—F1	1.8566 (10)	Cr2—N4ⁱⁱ	2.0800 (17)
Cr1—N1ⁱ	2.0867 (16)	Cr2—N3ⁱⁱ	2.0908 (14)
Cr1—N1	2.0867 (16)	Cr2—N3	2.0908 (14)
Cr1—N2ⁱ	2.0929 (15)	N3—C11	1.345 (2)
Cr1—N2	2.0929 (15)	N3—C15	1.350 (2)
N1—C1	1.3478 (19)	C11—C12	1.385 (2)
N1—C5	1.348 (2)	C11—H11	0.9500
C1—C2	1.386 (2)	C12—C13	1.383 (2)
C1—H1	0.9500	C12—H12	0.9500
C2—C3	1.384 (2)	C13—C14	1.386 (3)
C2—H2	0.9500	C13—H13	0.9500
C3—C4	1.396 (2)	C14—C15	1.385 (2)
C3—H3	0.9500	C14—H14	0.9500
C4—C5	1.386 (2)	C15—H15	0.9500
C4—H4	0.9500	N4—C16	1.341 (2)
C5—H5	0.9500	N4—C20	1.348 (2)
N2—C6	1.343 (2)	C16—C17	1.387 (2)
N2—C10	1.350 (2)	C16—H16	0.9500
C6—C7	1.388 (2)	C17—C18	1.382 (3)
C6—H6	0.9500	C17—H17	0.9500
C7—C8	1.383 (2)	C18—C19	1.391 (3)
C7—H7	0.9500	C18—H18	0.9500
C8—C9	1.386 (3)	C19—C20	1.378 (3)
C8—H8	0.9500	C19—H19	0.9500
C9—C10	1.381 (2)	C20—H20	0.9500
C9—H9	0.9500	Cl1P—O4P	1.4342 (15)
C10—H10	0.9500	Cl1P—O3P	1.4342 (14)
Cr2—F2ⁱⁱ	1.8552 (10)	Cl1P—O2P	1.4351 (15)
Cr2—F2	1.8552 (10)	Cl1P—O1P	1.4416 (14)

F1ⁱ—Cr1—F1	180.0	F2ⁱⁱ—Cr2—N4ⁱⁱ	90.36 (6)
F1ⁱ—Cr1—N1ⁱ	90.52 (5)	F2—Cr2—N4ⁱⁱ	89.64 (6)
F1—Cr1—N1ⁱ	89.48 (5)	N4—Cr2—N4ⁱⁱ	180.0
F1ⁱ—Cr1—N1	89.48 (5)	F2ⁱⁱ—Cr2—N3ⁱⁱ	90.31 (5)
F1—Cr1—N1	90.52 (5)	F2—Cr2—N3ⁱⁱ	89.69 (5)
N1ⁱ—Cr1—N1	180.00 (7)	N4—Cr2—N3ⁱⁱ	87.08 (6)
F1ⁱ—Cr1—N2ⁱ	90.40 (5)	N4ⁱⁱ—Cr2—N3ⁱⁱ	92.92 (6)
F1—Cr1—N2ⁱ	89.60 (5)	F2ⁱⁱ—Cr2—N3	89.68 (5)
N1ⁱ—Cr1—N2ⁱ	92.68 (6)	F2—Cr2—N3	90.32 (5)
N1—Cr1—N2ⁱ	87.32 (6)	N4—Cr2—N3	92.92 (6)
F1ⁱ—Cr1—N2	89.60 (5)	N4ⁱⁱ—Cr2—N3	87.08 (6)
F1—Cr1—N2	90.40 (5)	N3ⁱⁱ—Cr2—N3	180.0
N1ⁱ—Cr1—N2	87.32 (6)	C11—N3—C15	118.33 (14)
N1—Cr1—N2	92.68 (6)	C11—N3—Cr2	120.91 (11)
N2ⁱ—Cr1—N2	180.0	C15—N3—Cr2	120.55 (11)
C1—N1—C5	118.53 (14)	N3—C11—C12	122.38 (15)
C1—N1—Cr1	119.68 (11)	N3—C11—H11	118.8
C5—N1—Cr1	121.77 (11)	C12—C11—H11	118.8
N1—C1—C2	122.25 (15)	C13—C12—C11	119.25 (16)
N1—C1—H1	118.9	C13—C12—H12	120.4
C2—C1—H1	118.9	C11—C12—H12	120.4
C3—C2—C1	119.33 (15)	C12—C13—C14	118.63 (15)
C3—C2—H2	120.3	C12—C13—H13	120.7
C1—C2—H2	120.3	C14—C13—H13	120.7
C2—C3—C4	118.55 (15)	C15—C14—C13	119.30 (15)
C2—C3—H3	120.7	C15—C14—H14	120.4
C4—C3—H3	120.7	C13—C14—H14	120.4
C5—C4—C3	119.09 (16)	N3—C15—C14	122.11 (15)
C5—C4—H4	120.5	N3—C15—H15	118.9
C3—C4—H4	120.5	C14—C15—H15	118.9
N1—C5—C4	122.22 (15)	C16—N4—C20	118.68 (15)
N1—C5—H5	118.9	C16—N4—Cr2	120.86 (11)
C4—C5—H5	118.9	C20—N4—Cr2	120.25 (12)
C6—N2—C10	118.41 (14)	N4—C16—C17	122.13 (16)
C6—N2—Cr1	120.40 (10)	N4—C16—H16	118.9
C10—N2—Cr1	121.05 (11)	C17—C16—H16	118.9
N2—C6—C7	122.17 (15)	C18—C17—C16	119.13 (17)
N2—C6—H6	118.9	C18—C17—H17	120.4
C7—C6—H6	118.9	C16—C17—H17	120.4
C8—C7—C6	119.12 (16)	C17—C18—C19	118.76 (17)
C8—C7—H7	120.4	C17—C18—H18	120.6
C6—C7—H7	120.4	C19—C18—H18	120.6
C7—C8—C9	118.91 (16)	C20—C19—C18	119.08 (17)
C7—C8—H8	120.5	C20—C19—H19	120.5
C9—C8—H8	120.5	C18—C19—H19	120.5
C10—C9—C8	119.00 (15)	N4—C20—C19	122.20 (17)
C10—C9—H9	120.5	N4—C20—H20	118.9
C8—C9—H9	120.5	C19—C20—H20	118.9
N2—C10—C9	122.39 (16)	O4P—Cl1P—O3P	110.13 (10)
N2—C10—H10	118.8	O4P—Cl1P—O2P	109.84 (11)
C9—C10—H10	118.8	O3P—Cl1P—O2P	109.44 (9)
F2ⁱⁱ—Cr2—F2	180.0	O4P—Cl1P—O1P	109.02 (9)
F2ⁱⁱ—Cr2—N4	89.64 (6)	O3P—Cl1P—O1P	108.90 (9)
F2—Cr2—N4	90.36 (6)	O2P—Cl1P—O1P	109.50 (10)

C5—N1—C1—C2	1.2 (2)	C15—N3—C11—C12	−0.1 (2)
Cr1—N1—C1—C2	179.81 (12)	Cr2—N3—C11—C12	−175.00 (12)
N1—C1—C2—C3	0.3 (2)	N3—C11—C12—C13	−0.4 (3)
C1—C2—C3—C4	−1.2 (2)	C11—C12—C13—C14	0.4 (3)
C2—C3—C4—C5	0.5 (3)	C12—C13—C14—C15	0.0 (2)
C1—N1—C5—C4	−1.9 (2)	C11—N3—C15—C14	0.5 (2)
Cr1—N1—C5—C4	179.55 (13)	Cr2—N3—C15—C14	175.44 (12)
C3—C4—C5—N1	1.0 (3)	C13—C14—C15—N3	−0.5 (2)
C10—N2—C6—C7	0.4 (2)	C20—N4—C16—C17	−0.9 (2)
Cr1—N2—C6—C7	−175.43 (12)	Cr2—N4—C16—C17	173.85 (12)
N2—C6—C7—C8	−0.6 (3)	N4—C16—C17—C18	0.9 (2)
C6—C7—C8—C9	0.4 (3)	C16—C17—C18—C19	0.1 (2)
C7—C8—C9—C10	0.0 (3)	C17—C18—C19—C20	−1.2 (3)
C6—N2—C10—C9	0.1 (2)	C16—N4—C20—C19	−0.3 (2)
Cr1—N2—C10—C9	175.84 (12)	Cr2—N4—C20—C19	−175.00 (14)
C8—C9—C10—N2	−0.2 (3)	C18—C19—C20—N4	1.3 (3)

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1···F1	0.95	2.36	2.892 (2)	115
C6—H6···F1	0.95	2.31	2.874 (2)	118
C11—H11···F2	0.95	2.32	2.879 (2)	117
C16—H16···F2	0.95	2.39	2.915 (2)	115
C14—H14···O1P	0.95	2.61	3.154 (2)	117
C9—H9···O2P	0.95	2.63	3.320 (3)	130
C1—H1···O3Pⁱⁱⁱ	0.95	2.41	3.107 (2)	130
C4—H4···O1P^iv	0.95	2.51	3.368 (2)	150
C5—H5···F1ⁱ	0.95	2.38	2.900 (2)	114
C10—H10···F1ⁱ	0.95	2.31	2.863 (2)	117
C15—H15···F2ⁱⁱ	0.95	2.29	2.856 (2)	117
C20—H20···F2ⁱⁱ	0.95	2.34	2.860 (2)	114
C15—H15···O3P^v	0.95	2.64	3.466 (2)	146
C19—H19···O2P^vi	0.95	2.58	3.227 (3)	125

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C1—H1···F1	0.95	2.36	2.892 (2)	115
C6—H6···F1	0.95	2.31	2.874 (2)	118
C11—H11···F2	0.95	2.32	2.879 (2)	117
C16—H16···F2	0.95	2.39	2.915 (2)	115
C14—H14···O1P	0.95	2.61	3.154 (2)	117
C9—H9···O2P	0.95	2.63	3.320 (3)	130
C1—H1···O3Pⁱ	0.95	2.41	3.107 (2)	130
C4—H4···O1Pⁱⁱ	0.95	2.51	3.368 (2)	150
C5—H5···F1ⁱⁱⁱ	0.95	2.38	2.900 (2)	114
C10—H10···F1ⁱⁱⁱ	0.95	2.31	2.863 (2)	117
C15—H15···F2^iv	0.95	2.29	2.856 (2)	117
C20—H20···F2^iv	0.95	2.34	2.860 (2)	114
C15—H15···O3P^v	0.95	2.64	3.466 (2)	146
C19—H19···O2P^vi	0.95	2.58	3.227 (3)	125

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

Acknowledgements

This work was supported by a grant from the 2012 Academic Research Fund of Andong National University. The experiment at the PLS-II 2D-SMC beamline was supported in part by MEST and POSTECH.

References

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

trans-Di­fluorido­tetra­kis­(pyridine-κN)chromium(III) perchlorate from synchrotron radiation

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metal-organic compounds

trans-Difluoridotetrakis(pyridine-κN)chromium(III) perchlorate from synchrotron radiation